#------------------------------------------------------------------------------
#$Date: 2019-11-07 22:50:16 +0200 (Thu, 07 Nov 2019) $
#$Revision: 223870 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/12/1551215.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1551215
loop_
_publ_author_name
'Ding, Qing-Rong'
'Xu, Gui-Lan'
'Zhang, Lei'
'Zhang, Jian'
_publ_section_title
;
Ligand-directed assembly engineering of trapezoidal {Ti5}
building blocks stabilized by dimethylglyoxime.
;
_journal_issue 27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first 9916
_journal_page_last 9919
_journal_paper_doi 10.1039/c9dt02032b
_journal_volume 48
_journal_year 2019
_chemical_formula_moiety 'C82 H170 N4 O36 Ti10'
_chemical_formula_sum 'C82 H170 N4 O36 Ti10'
_chemical_formula_weight 2266.90
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_Hall '-P 2yn'
_space_group_name_H-M_alt 'P 1 21/n 1'
_symmetry_space_group_name_Hall '-P 2yn'
_symmetry_space_group_name_H-M 'P 1 21/n 1'
_atom_sites_solution_hydrogens geom
_audit_creation_method SHELXL-2014
_audit_update_record
;
2019-05-29 deposited with the CCDC. 2019-06-04 downloaded from the CCDC.
;
_cell_angle_alpha 90
_cell_angle_beta 92.241(2)
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 10.9245(2)
_cell_length_b 23.0505(6)
_cell_length_c 23.9209(6)
_cell_measurement_reflns_used 8489
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 74.1030
_cell_measurement_theta_min 3.6810
_cell_volume 6019.0(2)
_computing_cell_refinement 'Bruker FRAMBO'
_computing_data_collection 'Bruker FRAMBO'
_computing_data_reduction 'Bruker SAINT'
_computing_molecular_graphics 'Bruker SHELXTL'
_computing_publication_material 'Bruker SHELXTL'
_computing_structure_refinement 'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution 'Bruker SHELXTL'
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean 10.3503
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.0306
_diffrn_reflns_av_unetI/netI 0.0422
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max 8
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 28
_diffrn_reflns_limit_k_min -23
_diffrn_reflns_limit_l_max 29
_diffrn_reflns_limit_l_min -28
_diffrn_reflns_number 25032
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full 67.679
_diffrn_reflns_theta_max 74.332
_diffrn_reflns_theta_min 3.698
_diffrn_source 'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu 5.919
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.38664
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.251
_exptl_crystal_description block
_exptl_crystal_F_000 2396
_exptl_crystal_size_max 0.5
_exptl_crystal_size_mid 0.3
_exptl_crystal_size_min 0.1
_refine_diff_density_max 0.796
_refine_diff_density_min -0.553
_refine_diff_density_rms 0.076
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.032
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 595
_refine_ls_number_reflns 11931
_refine_ls_number_restraints 95
_refine_ls_restrained_S_all 1.089
_refine_ls_R_factor_all 0.0955
_refine_ls_R_factor_gt 0.0691
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1530P)^2^+0.4080P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.2097
_refine_ls_wR_factor_ref 0.2353
_reflns_Friedel_coverage 0.000
_reflns_number_gt 8166
_reflns_number_total 11931
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file c9dt02032b2.cif
_cod_data_source_block a
_cod_depositor_comments
'Adding full bibliography for 1551215--1551222.cif.'
_cod_database_code 1551215
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.528
_oxdiff_exptl_absorpt_empirical_full_max 1.926
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelxl_version_number 2014-3
_shelx_res_file
;
TITL a_a.res in P2(1)/n
REM Old TITL a in P2(1)/n
REM SHELXT solution in P2(1)/n
REM R1 0.207, Rweak 0.014, Alpha 0.055, Orientation as input
REM Formula found by SHELXT: C33 N6 O16 Ti5
CELL 1.54178 10.9245 23.0505 23.9209 90 92.241 90
ZERR 2 0.0002 0.0006 0.0006 0 0.002 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H N O Ti
UNIT 164 340 8 72 20
DFIX 1.52 0.01 C8 C10
DFIX 1.52 0.01 C33 C35
DFIX 1.52 0.01 C27 C28
DFIX 1.52 0.01 C11 C12
DFIX 1.52 0.01 C28 C29
DELU C8 C9
DELU C8 C10
DELU C27 C28
DELU C33 C35
DELU C39 C40
DELU 0.02 0.01 O15 C8
SIMU 0.01 0.02 2 C8 C10 C9 C15
SIMU 0.01 0.02 2 C11 C12 C13 O9
SIMU 0.01 0.02 2 C28 C27 C29 O3
SIMU 0.01 0.02 2 O15 Ti5 C8
SIMU 0.01 0.02 2 C33 O5 C34 C35
ISOR C29
L.S. 60
PLAN 20
BOND $H
list 4
fmap 2
acta
REM
REM
REM
WGHT 0.153000 0.408000
FVAR 0.29143
TI3 5 0.442736 0.318314 0.657862 11.00000 0.05044 0.05118 =
0.05216 0.01103 -0.00401 -0.00240
TI2 5 0.196735 0.386190 0.664727 11.00000 0.04332 0.07638 =
0.06102 0.01859 0.00001 -0.00068
TI1 5 0.401572 0.447754 0.738848 11.00000 0.06103 0.06637 =
0.07250 -0.00453 0.00446 0.00166
TI4 5 0.261599 0.266909 0.566324 11.00000 0.07839 0.06656 =
0.07093 0.00559 -0.01871 -0.01350
TI5 5 0.523075 0.212376 0.551460 11.00000 0.09694 0.07036 =
0.08138 -0.01338 0.00977 -0.00448
O6 4 0.361771 0.377241 0.701037 11.00000 0.04261 0.06343 =
0.05784 0.00696 -0.00069 -0.00087
O12 4 0.475281 0.381813 0.599395 11.00000 0.05258 0.06004 =
0.06618 0.02160 0.00612 0.00109
O11 4 0.301302 0.433243 0.601577 11.00000 0.05197 0.06845 =
0.06686 0.02483 0.00666 0.00439
O7 4 0.260252 0.317964 0.628646 11.00000 0.05384 0.06715 =
0.06003 0.01506 -0.00741 -0.00738
O00A 4 0.450402 0.265679 0.711738 11.00000 0.07967 0.06438 =
0.06110 0.02054 -0.00524 0.00015
O5 4 0.232567 0.461726 0.708860 11.00000 0.06277 0.08456 =
0.08458 0.00245 0.00840 0.02021
O8 4 0.426843 0.263250 0.593816 11.00000 0.07311 0.06483 =
0.06570 -0.00616 -0.00776 -0.00443
O10 4 0.064101 0.407557 0.622995 11.00000 0.05238 0.09719 =
0.07879 0.02883 -0.00293 0.00114
O00E 4 0.115665 0.351485 0.720110 11.00000 0.04795 0.11717 =
0.07362 0.03249 0.00524 -0.00362
O2 4 0.649086 0.239147 0.605666 11.00000 0.07776 0.08340 =
0.09695 -0.01788 0.00482 0.01539
N1 3 0.592217 0.369816 0.702407 11.00000 0.05209 0.06550 =
0.07838 -0.00716 -0.00713 0.00164
N2 3 0.632095 0.287241 0.637221 11.00000 0.06615 0.06233 =
0.06713 0.00547 0.00256 0.00919
O9 4 0.352310 0.207427 0.518192 11.00000 0.11929 0.09385 =
0.08235 -0.02922 -0.01045 -0.01665
O1 4 0.566636 0.416832 0.732439 11.00000 0.05183 0.09926 =
0.15401 -0.05274 -0.01468 0.00327
O14 4 0.140183 0.218460 0.583455 11.00000 0.09065 0.07965 =
0.12994 0.00700 -0.01717 -0.02466
O13 4 0.208640 0.311550 0.509280 11.00000 0.14413 0.09065 =
0.07373 0.01000 -0.02950 -0.00327
O4 4 0.385008 0.442272 0.811755 11.00000 0.09833 0.14117 =
0.07408 -0.00671 0.00012 0.00960
C24 1 0.455457 0.463529 0.540991 11.00000 0.04910 0.05544 =
0.05297 0.01318 0.00054 -0.00010
O3 4 0.459192 0.518228 0.725459 11.00000 0.09890 0.07767 =
0.19460 0.01558 0.01691 -0.01129
C25 1 0.572251 0.455780 0.521810 11.00000 0.05430 0.06112 =
0.07092 0.02213 0.00495 0.00659
AFIX 43
H25 2 0.621335 0.426061 0.536458 11.00000 -1.20000
AFIX 0
C23 1 0.405836 0.423707 0.584056 11.00000 0.05283 0.05420 =
0.05493 0.01438 -0.00149 0.00022
C3 1 0.707109 0.357287 0.697450 11.00000 0.04710 0.08271 =
0.09995 -0.00819 -0.00827 0.00112
C26 1 0.616444 0.491709 0.481201 11.00000 0.04921 0.06663 =
0.06573 0.02053 0.00749 0.00375
AFIX 43
H26 2 0.694950 0.485955 0.468558 11.00000 -1.20000
AFIX 0
O16 4 0.602288 0.236550 0.492549 11.00000 0.13304 0.19992 =
0.08642 -0.02152 0.02110 -0.05954
O15 4 0.550719 0.138457 0.565277 11.00000 0.15109 0.07075 =
0.17021 -0.02146 -0.00410 0.01053
C1 1 0.729321 0.307817 0.662675 11.00000 0.05129 0.07814 =
0.08542 0.00428 -0.00151 0.00664
C30 1 0.009919 0.428715 0.572319 11.00000 0.07429 0.13528 =
0.09325 0.04870 -0.02102 -0.00472
AFIX 13
H30 2 0.074659 0.440393 0.547418 11.00000 -1.20000
AFIX 0
C4 1 0.807603 0.392169 0.725788 11.00000 0.05605 0.14577 =
0.21132 -0.07495 -0.02340 -0.00434
AFIX 33
H4A 2 0.885567 0.376055 0.716998 11.00000 -1.50000
H4B 2 0.802871 0.431594 0.712950 11.00000 -1.50000
H4C 2 0.798643 0.391167 0.765539 11.00000 -1.50000
AFIX 0
C36 1 0.151494 0.326249 0.772431 11.00000 0.07193 0.14955 =
0.08300 0.05651 0.00378 -0.00782
AFIX 13
H36 2 0.240689 0.329940 0.777018 11.00000 -1.20000
AFIX 0
C2 1 0.855043 0.281581 0.657939 11.00000 0.06405 0.11900 =
0.13243 -0.01829 -0.00552 0.02427
AFIX 33
H2A 2 0.913451 0.303649 0.680147 11.00000 -1.50000
H2B 2 0.854199 0.242252 0.671121 11.00000 -1.50000
H2C 2 0.877460 0.282152 0.619537 11.00000 -1.50000
AFIX 0
C17 1 0.232503 0.355105 0.469576 11.00000 0.18983 0.10597 =
0.07695 0.01539 -0.03961 -0.00827
AFIX 13
H17 2 0.224715 0.393189 0.487297 11.00000 -1.20000
AFIX 0
C14 1 0.103427 0.181057 0.625140 11.00000 0.08740 0.09869 =
0.16867 0.01823 0.01228 -0.01270
AFIX 13
H14 2 0.067264 0.204700 0.654277 11.00000 -1.20000
AFIX 0
C20 1 0.494274 0.235377 0.758974 11.00000 0.22560 0.14505 =
0.08890 0.05811 -0.01193 0.06448
AFIX 13
H20 2 0.419012 0.213468 0.764917 11.00000 -1.20000
AFIX 0
C33 1 0.163149 0.514562 0.710980 11.00000 0.13456 0.11913 =
0.13662 0.01331 0.02543 0.06795
AFIX 13
H33 2 0.091375 0.497734 0.691187 11.00000 -1.20000
AFIX 0
C31 1 -0.066410 0.383786 0.544483 11.00000 0.13859 0.17388 =
0.13959 0.00761 -0.06066 -0.01090
AFIX 33
H31A 2 -0.102234 0.399011 0.510257 11.00000 -1.50000
H31B 2 -0.016572 0.350762 0.536388 11.00000 -1.50000
H31C 2 -0.130190 0.372289 0.568657 11.00000 -1.50000
AFIX 0
C18 1 0.362635 0.347760 0.451183 11.00000 0.16945 0.16683 =
0.11815 0.01451 -0.00301 -0.03678
AFIX 33
H18A 2 0.380350 0.377068 0.424156 11.00000 -1.50000
H18B 2 0.418380 0.351457 0.483014 11.00000 -1.50000
H18C 2 0.371689 0.310099 0.434717 11.00000 -1.50000
AFIX 0
C11 1 0.293759 0.172420 0.474042 11.00000 0.18844 0.14305 =
0.12684 -0.06853 -0.01138 -0.03293
AFIX 13
H11 2 0.211817 0.187905 0.464997 11.00000 -1.20000
AFIX 0
C5 1 0.708581 0.266705 0.475860 11.00000 0.14583 0.26270 =
0.14869 0.04438 0.05042 -0.02818
AFIX 13
H5 2 0.740917 0.286013 0.509822 11.00000 -1.20000
AFIX 0
C38 1 0.094504 0.362125 0.818909 11.00000 0.17943 0.27397 =
0.08011 0.04350 0.02853 0.03591
AFIX 33
H38A 2 0.117650 0.345757 0.854681 11.00000 -1.50000
H38B 2 0.123368 0.401397 0.817187 11.00000 -1.50000
H38C 2 0.006893 0.361632 0.813892 11.00000 -1.50000
AFIX 0
C34 1 0.185302 0.555537 0.667015 11.00000 0.13709 0.09784 =
0.19714 0.04838 0.01309 0.04018
AFIX 33
H34A 2 0.229360 0.536788 0.638137 11.00000 -1.50000
H34B 2 0.108508 0.569727 0.651662 11.00000 -1.50000
H34C 2 0.232796 0.587391 0.681957 11.00000 -1.50000
AFIX 0
C15 1 0.212408 0.150314 0.651307 11.00000 0.12458 0.14144 =
0.16287 0.05251 -0.00473 0.01625
AFIX 33
H15A 2 0.185934 0.124618 0.680015 11.00000 -1.50000
H15B 2 0.252488 0.128354 0.623242 11.00000 -1.50000
H15C 2 0.268502 0.178308 0.667397 11.00000 -1.50000
AFIX 0
C19 1 0.136459 0.349871 0.422361 11.00000 0.25909 0.17339 =
0.09741 0.03064 -0.08399 0.00552
AFIX 33
H19A 2 0.150500 0.379038 0.394691 11.00000 -1.50000
H19B 2 0.141539 0.312142 0.405615 11.00000 -1.50000
H19C 2 0.056520 0.355118 0.436880 11.00000 -1.50000
AFIX 0
C28 1 0.548521 0.554203 0.702374 11.00000 0.15876 0.10421 =
0.25865 0.00200 0.05992 -0.02897
AFIX 13
H28 2 0.604127 0.547392 0.734853 11.00000 -1.20000
AFIX 0
C16 1 0.007917 0.141002 0.603284 11.00000 0.13792 0.14069 =
0.28842 0.05630 -0.03183 -0.07850
AFIX 33
H16A 2 -0.016182 0.115574 0.632675 11.00000 -1.50000
H16B 2 -0.061806 0.162863 0.589611 11.00000 -1.50000
H16C 2 0.039523 0.118476 0.573330 11.00000 -1.50000
AFIX 0
C32 1 -0.070246 0.480479 0.583484 11.00000 0.18577 0.20206 =
0.17708 0.03976 -0.07641 0.08547
AFIX 33
H32A 2 -0.106418 0.494404 0.548808 11.00000 -1.50000
H32B 2 -0.133753 0.469287 0.607931 11.00000 -1.50000
H32C 2 -0.021531 0.510655 0.600812 11.00000 -1.50000
AFIX 0
C39 1 0.422135 0.458165 0.864205 11.00000 0.17291 0.39359 =
0.09041 -0.08397 -0.02583 0.01662
C6 1 0.693287 0.309852 0.437270 11.00000 0.21315 0.20154 =
0.15967 0.01587 0.03600 -0.04516
AFIX 33
H6A 2 0.771445 0.326542 0.429732 11.00000 -1.50000
H6B 2 0.656977 0.294160 0.403344 11.00000 -1.50000
H6C 2 0.640667 0.339247 0.451550 11.00000 -1.50000
AFIX 0
C22 1 0.493354 0.267336 0.809193 11.00000 0.36740 0.31598 =
0.07276 0.01258 -0.03514 0.19113
AFIX 33
H22A 2 0.433982 0.297940 0.805519 11.00000 -1.50000
H22B 2 0.472421 0.242141 0.839314 11.00000 -1.50000
H22C 2 0.573031 0.283692 0.816949 11.00000 -1.50000
AFIX 0
C37 1 0.122490 0.264288 0.770443 11.00000 0.29248 0.13029 =
0.14613 0.07653 -0.07863 -0.03534
AFIX 33
H37A 2 0.146264 0.246681 0.805581 11.00000 -1.50000
H37B 2 0.036018 0.259282 0.763408 11.00000 -1.50000
H37C 2 0.166163 0.246251 0.741035 11.00000 -1.50000
AFIX 0
C21 1 0.567581 0.187394 0.747231 11.00000 0.37998 0.18213 =
0.18097 0.07549 -0.02811 0.16116
AFIX 33
H21A 2 0.594035 0.168951 0.781600 11.00000 -1.50000
H21B 2 0.521155 0.160343 0.724441 11.00000 -1.50000
H21C 2 0.637805 0.199997 0.727600 11.00000 -1.50000
AFIX 0
C8 1 0.629801 0.092952 0.588596 11.00000 0.21882 0.10822 =
0.24519 -0.00933 0.04375 0.03847
AFIX 13
H8 2 0.689930 0.105927 0.617403 11.00000 -1.20000
AFIX 0
C7 1 0.798490 0.222165 0.463747 11.00000 0.18844 0.23858 =
0.31492 0.07865 0.08586 -0.00890
AFIX 33
H7A 2 0.801825 0.194132 0.493446 11.00000 -1.50000
H7B 2 0.775270 0.203273 0.429172 11.00000 -1.50000
H7C 2 0.877584 0.239759 0.460644 11.00000 -1.50000
AFIX 0
C41 1 0.542008 0.451409 0.879615 11.00000 0.22841 0.42329 =
0.22410 -0.02434 -0.11314 0.03880
AFIX 33
H41A 2 0.555590 0.464283 0.917518 11.00000 -1.50000
H41B 2 0.563943 0.411210 0.876864 11.00000 -1.50000
H41C 2 0.591390 0.473951 0.855378 11.00000 -1.50000
AFIX 0
C40 1 0.329328 0.468567 0.903788 11.00000 0.33447 0.31914 =
0.10839 -0.04001 0.07229 -0.03737
AFIX 33
H40A 2 0.367230 0.479445 0.939128 11.00000 -1.50000
H40B 2 0.276633 0.499307 0.890401 11.00000 -1.50000
H40C 2 0.282001 0.433913 0.908329 11.00000 -1.50000
AFIX 0
C29 1 0.531017 0.614616 0.719648 11.00000 0.27024 0.14313 =
0.35857 -0.01657 0.08691 -0.07324
AFIX 33
H29A 2 0.592394 0.638591 0.703646 11.00000 -1.50000
H29B 2 0.451234 0.627609 0.706898 11.00000 -1.50000
H29C 2 0.537971 0.617175 0.759703 11.00000 -1.50000
AFIX 0
C12 1 0.367901 0.176275 0.424633 11.00000 0.27085 0.29345 =
0.15355 -0.11473 0.03244 -0.09934
AFIX 33
H12A 2 0.330836 0.153455 0.394971 11.00000 -1.50000
H12B 2 0.372786 0.216008 0.412901 11.00000 -1.50000
H12C 2 0.448785 0.161893 0.433569 11.00000 -1.50000
AFIX 0
C35 1 0.102646 0.519043 0.763059 11.00000 0.29732 0.19939 =
0.24818 0.02061 0.13887 0.12245
AFIX 33
H35A 2 0.056807 0.554553 0.763709 11.00000 -1.50000
H35B 2 0.048073 0.486752 0.766790 11.00000 -1.50000
H35C 2 0.162629 0.518819 0.793477 11.00000 -1.50000
AFIX 0
C13 1 0.282677 0.110318 0.493665 11.00000 0.31683 0.18218 =
0.22883 -0.07347 -0.06865 -0.06665
AFIX 33
H13A 2 0.244071 0.087395 0.464474 11.00000 -1.50000
H13B 2 0.362782 0.095064 0.502728 11.00000 -1.50000
H13C 2 0.234146 0.109086 0.526245 11.00000 -1.50000
AFIX 0
C9 1 0.678890 0.064105 0.543799 11.00000 0.32434 0.17994 =
0.31314 -0.02127 0.07971 0.08746
AFIX 33
H9A 2 0.731855 0.033608 0.557506 11.00000 -1.50000
H9B 2 0.613849 0.047821 0.520650 11.00000 -1.50000
H9C 2 0.724950 0.090913 0.522229 11.00000 -1.50000
AFIX 0
C27 1 0.637100 0.529401 0.665421 11.00000 0.23215 0.21503 =
0.31084 0.03316 0.11344 -0.00747
AFIX 33
H27A 2 0.691203 0.559307 0.653326 11.00000 -1.50000
H27B 2 0.683752 0.499991 0.685074 11.00000 -1.50000
H27C 2 0.594865 0.512521 0.633449 11.00000 -1.50000
AFIX 0
C10 1 0.547608 0.045689 0.606217 11.00000 0.31108 0.19783 =
0.35504 0.08050 0.11649 0.02882
AFIX 33
H10A 2 0.503859 0.058075 0.638140 11.00000 -1.50000
H10B 2 0.490331 0.036457 0.576069 11.00000 -1.50000
H10C 2 0.595440 0.011948 0.615846 11.00000 -1.50000
AFIX 0
HKLF 4
REM a_a.res in P2(1)/n
REM R1 = 0.0691 for 8166 Fo > 4sig(Fo) and 0.0955 for all 11931 data
REM 595 parameters refined using 95 restraints
END
WGHT 0.1483 0.4332
REM Highest difference peak 0.796, deepest hole -0.553, 1-sigma level 0.076
Q1 1 0.6558 0.5581 0.7573 11.00000 0.05 0.80
Q2 1 0.0430 0.5106 0.7257 11.00000 0.05 0.77
Q3 1 0.1777 0.1879 0.4497 11.00000 0.05 0.58
Q4 1 0.1907 0.1945 0.4382 11.00000 0.05 0.54
Q5 1 0.6660 0.0810 0.6419 11.00000 0.05 0.53
Q6 1 0.3965 0.1236 0.4561 11.00000 0.05 0.51
Q7 1 0.3234 0.2417 0.5589 11.00000 0.05 0.51
Q8 1 0.4150 0.2016 0.7892 11.00000 0.05 0.38
Q9 1 0.4660 0.5966 0.6686 11.00000 0.05 0.37
Q10 1 0.3040 0.3776 0.7005 11.00000 0.05 0.36
Q11 1 0.1875 0.5400 0.7588 11.00000 0.05 0.36
Q12 1 0.2085 0.3553 0.6437 11.00000 0.05 0.35
Q13 1 0.4683 0.3881 0.8932 11.00000 0.05 0.34
Q14 1 0.5649 0.0784 0.5628 11.00000 0.05 0.33
Q15 1 0.4607 0.1842 0.7733 11.00000 0.05 0.32
Q16 1 0.4267 0.3977 0.9062 11.00000 0.05 0.31
Q17 1 0.4670 0.5008 0.6886 11.00000 0.05 0.30
Q18 1 0.6330 0.2505 0.7838 11.00000 0.05 0.27
Q19 1 0.6571 0.2504 0.4381 11.00000 0.05 0.27
Q20 1 0.5161 0.5687 0.6741 11.00000 0.05 0.26
;
_shelx_res_checksum 62141
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Ti3 Ti 0.44274(6) 0.31831(3) 0.65786(3) 0.05142(19) Uani 1 1 d . .
Ti2 Ti 0.19673(6) 0.38619(4) 0.66473(3) 0.0603(2) Uani 1 1 d . .
Ti1 Ti 0.40157(7) 0.44775(4) 0.73885(4) 0.0666(2) Uani 1 1 d . .
Ti4 Ti 0.26160(8) 0.26691(4) 0.56632(4) 0.0725(3) Uani 1 1 d . .
Ti5 Ti 0.52307(10) 0.21238(4) 0.55146(4) 0.0827(3) Uani 1 1 d . U
O6 O 0.3618(2) 0.37724(12) 0.70104(11) 0.0547(6) Uani 1 1 d . .
O12 O 0.4753(2) 0.38181(12) 0.59939(12) 0.0595(7) Uani 1 1 d . .
O11 O 0.3013(2) 0.43324(13) 0.60158(12) 0.0623(7) Uani 1 1 d . .
O7 O 0.2603(2) 0.31796(13) 0.62865(12) 0.0606(7) Uani 1 1 d . .
O00A O 0.4504(3) 0.26568(13) 0.71174(13) 0.0686(7) Uani 1 1 d . .
O5 O 0.2326(3) 0.46173(16) 0.70886(15) 0.0772(9) Uani 1 1 d . U
O8 O 0.4268(3) 0.26325(14) 0.59382(13) 0.0682(7) Uani 1 1 d . .
O10 O 0.0641(3) 0.40756(16) 0.62299(14) 0.0763(9) Uani 1 1 d . .
O00E O 0.1157(2) 0.35148(17) 0.72011(14) 0.0795(10) Uani 1 1 d . .
O2 O 0.6491(3) 0.23915(17) 0.60567(17) 0.0860(10) Uani 1 1 d . .
N1 N 0.5922(3) 0.36982(17) 0.70241(17) 0.0656(9) Uani 1 1 d . .
N2 N 0.6321(3) 0.28724(16) 0.63722(16) 0.0652(9) Uani 1 1 d . .
O9 O 0.3523(4) 0.20743(19) 0.51819(17) 0.0989(12) Uani 1 1 d . U
O1 O 0.5666(3) 0.41683(18) 0.7324(2) 0.1022(14) Uani 1 1 d . .
O14 O 0.1402(4) 0.21846(18) 0.5835(2) 0.1006(13) Uani 1 1 d . .
O13 O 0.2086(5) 0.31155(19) 0.50928(17) 0.1037(13) Uani 1 1 d . .
O4 O 0.3850(4) 0.4423(2) 0.81175(17) 0.1046(13) Uani 1 1 d . .
C24 C 0.4555(3) 0.46353(17) 0.54099(16) 0.0525(8) Uani 1 1 d . .
O3 O 0.4592(4) 0.51823(19) 0.7255(3) 0.1234(17) Uani 1 1 d . U
C25 C 0.5723(4) 0.45578(19) 0.52181(19) 0.0620(10) Uani 1 1 d . .
H25 H 0.6213 0.4261 0.5365 0.074 Uiso 1 1 calc R U
C23 C 0.4058(3) 0.42371(17) 0.58406(16) 0.0541(8) Uani 1 1 d . .
C3 C 0.7071(4) 0.3573(2) 0.6974(2) 0.0769(13) Uani 1 1 d . .
C26 C 0.6164(3) 0.49171(19) 0.48120(18) 0.0604(10) Uani 1 1 d . .
H26 H 0.6950 0.4860 0.4686 0.072 Uiso 1 1 calc R U
O16 O 0.6023(5) 0.2365(3) 0.4925(2) 0.139(2) Uani 1 1 d . .
O15 O 0.5507(5) 0.1385(2) 0.5653(3) 0.1310(17) Uani 1 1 d . U
C1 C 0.7293(4) 0.3078(2) 0.6627(2) 0.0717(12) Uani 1 1 d . .
C30 C 0.0099(5) 0.4287(3) 0.5723(3) 0.102(2) Uani 1 1 d . .
H30 H 0.0747 0.4404 0.5474 0.122 Uiso 1 1 calc R U
C4 C 0.8076(5) 0.3922(4) 0.7258(4) 0.138(3) Uani 1 1 d . .
H4A H 0.8856 0.3761 0.7170 0.208 Uiso 1 1 calc R U
H4B H 0.8029 0.4316 0.7129 0.208 Uiso 1 1 calc R U
H4C H 0.7986 0.3912 0.7655 0.208 Uiso 1 1 calc R U
C36 C 0.1515(5) 0.3262(3) 0.7724(2) 0.101(2) Uani 1 1 d . .
H36 H 0.2407 0.3299 0.7770 0.122 Uiso 1 1 calc R U
C2 C 0.8550(5) 0.2816(3) 0.6579(3) 0.105(2) Uani 1 1 d . .
H2A H 0.9135 0.3036 0.6801 0.158 Uiso 1 1 calc R U
H2B H 0.8542 0.2423 0.6711 0.158 Uiso 1 1 calc R U
H2C H 0.8775 0.2822 0.6195 0.158 Uiso 1 1 calc R U
C17 C 0.2325(9) 0.3551(4) 0.4696(3) 0.125(3) Uani 1 1 d . .
H17 H 0.2247 0.3932 0.4873 0.151 Uiso 1 1 calc R U
C14 C 0.1034(6) 0.1811(3) 0.6251(4) 0.118(2) Uani 1 1 d . .
H14 H 0.0673 0.2047 0.6543 0.142 Uiso 1 1 calc R U
C20 C 0.4943(11) 0.2354(4) 0.7590(3) 0.154(4) Uani 1 1 d . .
H20 H 0.4190 0.2135 0.7649 0.184 Uiso 1 1 calc R U
C33 C 0.1631(8) 0.5146(4) 0.7110(4) 0.130(2) Uani 1 1 d D U
H33 H 0.0914 0.4977 0.6912 0.155 Uiso 1 1 calc R U
C31 C -0.0664(9) 0.3838(5) 0.5445(4) 0.152(4) Uani 1 1 d . .
H31A H -0.1022 0.3990 0.5103 0.229 Uiso 1 1 calc R U
H31B H -0.0166 0.3508 0.5364 0.229 Uiso 1 1 calc R U
H31C H -0.1302 0.3723 0.5687 0.229 Uiso 1 1 calc R U
C18 C 0.3626(10) 0.3478(5) 0.4512(4) 0.152(4) Uani 1 1 d . .
H18A H 0.3804 0.3771 0.4242 0.228 Uiso 1 1 calc R U
H18B H 0.4184 0.3515 0.4830 0.228 Uiso 1 1 calc R U
H18C H 0.3717 0.3101 0.4347 0.228 Uiso 1 1 calc R U
C11 C 0.2938(10) 0.1724(5) 0.4740(4) 0.153(3) Uani 1 1 d D U
H11 H 0.2118 0.1879 0.4650 0.184 Uiso 1 1 calc R U
C5 C 0.7086(11) 0.2667(7) 0.4759(5) 0.185(5) Uani 1 1 d . .
H5 H 0.7409 0.2860 0.5098 0.221 Uiso 1 1 calc R U
C38 C 0.0945(10) 0.3621(6) 0.8189(3) 0.177(5) Uani 1 1 d . .
H38A H 0.1177 0.3458 0.8547 0.266 Uiso 1 1 calc R U
H38B H 0.1234 0.4014 0.8172 0.266 Uiso 1 1 calc R U
H38C H 0.0069 0.3616 0.8139 0.266 Uiso 1 1 calc R U
C34 C 0.1853(8) 0.5555(3) 0.6670(4) 0.144(3) Uani 1 1 d . U
H34A H 0.2294 0.5368 0.6381 0.216 Uiso 1 1 calc R U
H34B H 0.1085 0.5697 0.6517 0.216 Uiso 1 1 calc R U
H34C H 0.2328 0.5874 0.6820 0.216 Uiso 1 1 calc R U
C15 C 0.2124(8) 0.1503(4) 0.6513(4) 0.143(3) Uani 1 1 d . .
H15A H 0.1859 0.1246 0.6800 0.215 Uiso 1 1 calc R U
H15B H 0.2525 0.1284 0.6232 0.215 Uiso 1 1 calc R U
H15C H 0.2685 0.1783 0.6674 0.215 Uiso 1 1 calc R U
C19 C 0.1365(12) 0.3499(5) 0.4224(3) 0.179(5) Uani 1 1 d . .
H19A H 0.1505 0.3790 0.3947 0.269 Uiso 1 1 calc R U
H19B H 0.1415 0.3121 0.4056 0.269 Uiso 1 1 calc R U
H19C H 0.0565 0.3551 0.4369 0.269 Uiso 1 1 calc R U
C28 C 0.5485(10) 0.5542(4) 0.7024(6) 0.173(3) Uani 1 1 d D U
H28 H 0.6041 0.5474 0.7349 0.207 Uiso 1 1 calc R U
C16 C 0.0079(9) 0.1410(4) 0.6033(6) 0.190(5) Uani 1 1 d . .
H16A H -0.0162 0.1156 0.6327 0.285 Uiso 1 1 calc R U
H16B H -0.0618 0.1629 0.5896 0.285 Uiso 1 1 calc R U
H16C H 0.0395 0.1185 0.5733 0.285 Uiso 1 1 calc R U
C32 C -0.0702(10) 0.4805(5) 0.5835(5) 0.190(5) Uani 1 1 d . .
H32A H -0.1064 0.4944 0.5488 0.286 Uiso 1 1 calc R U
H32B H -0.1338 0.4693 0.6079 0.286 Uiso 1 1 calc R U
H32C H -0.0215 0.5107 0.6008 0.286 Uiso 1 1 calc R U
C39 C 0.4221(12) 0.4582(8) 0.8642(4) 0.220(7) Uani 1 1 d . U
C6 C 0.6933(12) 0.3099(6) 0.4373(5) 0.191(5) Uani 1 1 d . .
H6A H 0.7714 0.3265 0.4297 0.286 Uiso 1 1 calc R U
H6B H 0.6570 0.2942 0.4033 0.286 Uiso 1 1 calc R U
H6C H 0.6407 0.3392 0.4516 0.286 Uiso 1 1 calc R U
C22 C 0.4934(15) 0.2673(7) 0.8092(4) 0.253(9) Uani 1 1 d . .
H22A H 0.4340 0.2979 0.8055 0.380 Uiso 1 1 calc R U
H22B H 0.4724 0.2421 0.8393 0.380 Uiso 1 1 calc R U
H22C H 0.5730 0.2837 0.8169 0.380 Uiso 1 1 calc R U
C37 C 0.1225(13) 0.2643(4) 0.7704(4) 0.192(6) Uani 1 1 d . .
H37A H 0.1463 0.2467 0.8056 0.288 Uiso 1 1 calc R U
H37B H 0.0360 0.2593 0.7634 0.288 Uiso 1 1 calc R U
H37C H 0.1662 0.2463 0.7410 0.288 Uiso 1 1 calc R U
C21 C 0.5676(15) 0.1874(5) 0.7472(5) 0.249(8) Uani 1 1 d . .
H21A H 0.5940 0.1690 0.7816 0.373 Uiso 1 1 calc R U
H21B H 0.5212 0.1603 0.7244 0.373 Uiso 1 1 calc R U
H21C H 0.6378 0.2000 0.7276 0.373 Uiso 1 1 calc R U
C8 C 0.6298(12) 0.0930(4) 0.5886(7) 0.190(3) Uani 1 1 d D U
H8 H 0.6899 0.1059 0.6174 0.228 Uiso 1 1 calc R U
C7 C 0.7985(13) 0.2222(7) 0.4637(7) 0.245(8) Uani 1 1 d . .
H7A H 0.8018 0.1941 0.4934 0.368 Uiso 1 1 calc R U
H7B H 0.7753 0.2033 0.4292 0.368 Uiso 1 1 calc R U
H7C H 0.8776 0.2398 0.4606 0.368 Uiso 1 1 calc R U
C41 C 0.5420(15) 0.4514(9) 0.8796(7) 0.295(11) Uani 1 1 d . .
H41A H 0.5556 0.4643 0.9175 0.443 Uiso 1 1 calc R U
H41B H 0.5639 0.4112 0.8769 0.443 Uiso 1 1 calc R U
H41C H 0.5914 0.4740 0.8554 0.443 Uiso 1 1 calc R U
C40 C 0.3293(15) 0.4686(7) 0.9038(5) 0.252(8) Uani 1 1 d . U
H40A H 0.3672 0.4794 0.9391 0.379 Uiso 1 1 calc R U
H40B H 0.2766 0.4993 0.8904 0.379 Uiso 1 1 calc R U
H40C H 0.2820 0.4339 0.9083 0.379 Uiso 1 1 calc R U
C29 C 0.5310(15) 0.6146(5) 0.7196(7) 0.255(6) Uani 1 1 d D U
H29A H 0.5924 0.6386 0.7036 0.383 Uiso 1 1 calc R U
H29B H 0.4512 0.6276 0.7069 0.383 Uiso 1 1 calc R U
H29C H 0.5380 0.6172 0.7597 0.383 Uiso 1 1 calc R U
C12 C 0.3679(13) 0.1763(7) 0.4246(5) 0.239(6) Uani 1 1 d D U
H12A H 0.3308 0.1535 0.3950 0.358 Uiso 1 1 calc R U
H12B H 0.3728 0.2160 0.4129 0.358 Uiso 1 1 calc R U
H12C H 0.4488 0.1619 0.4336 0.358 Uiso 1 1 calc R U
C35 C 0.1026(14) 0.5190(6) 0.7631(5) 0.245(6) Uani 1 1 d D U
H35A H 0.0568 0.5546 0.7637 0.367 Uiso 1 1 calc R U
H35B H 0.0481 0.4868 0.7668 0.367 Uiso 1 1 calc R U
H35C H 0.1626 0.5188 0.7935 0.367 Uiso 1 1 calc R U
C13 C 0.2827(16) 0.1103(6) 0.4937(6) 0.245(6) Uani 1 1 d . U
H13A H 0.2441 0.0874 0.4645 0.367 Uiso 1 1 calc R U
H13B H 0.3628 0.0951 0.5027 0.367 Uiso 1 1 calc R U
H13C H 0.2341 0.1091 0.5262 0.367 Uiso 1 1 calc R U
C9 C 0.6789(17) 0.0641(6) 0.5438(8) 0.271(7) Uani 1 1 d . U
H9A H 0.7319 0.0336 0.5575 0.406 Uiso 1 1 calc R U
H9B H 0.6138 0.0478 0.5207 0.406 Uiso 1 1 calc R U
H9C H 0.7250 0.0909 0.5222 0.406 Uiso 1 1 calc R U
C27 C 0.6371(14) 0.5294(6) 0.6654(7) 0.250(6) Uani 1 1 d D U
H27A H 0.6912 0.5593 0.6533 0.375 Uiso 1 1 calc R U
H27B H 0.6838 0.5000 0.6851 0.375 Uiso 1 1 calc R U
H27C H 0.5949 0.5125 0.6334 0.375 Uiso 1 1 calc R U
C10 C 0.5476(16) 0.0457(6) 0.6062(9) 0.285(7) Uani 1 1 d D U
H10A H 0.5039 0.0581 0.6381 0.428 Uiso 1 1 calc R U
H10B H 0.4903 0.0365 0.5761 0.428 Uiso 1 1 calc R U
H10C H 0.5954 0.0119 0.6158 0.428 Uiso 1 1 calc R U
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ti3 0.0504(3) 0.0512(4) 0.0522(4) 0.0110(3) -0.0040(3) -0.0024(3)
Ti2 0.0433(3) 0.0764(5) 0.0610(4) 0.0186(4) 0.0000(3) -0.0007(3)
Ti1 0.0610(4) 0.0664(5) 0.0725(5) -0.0045(4) 0.0045(3) 0.0017(3)
Ti4 0.0784(5) 0.0666(5) 0.0709(5) 0.0056(4) -0.0187(4) -0.0135(4)
Ti5 0.0969(6) 0.0704(5) 0.0814(6) -0.0134(5) 0.0098(5) -0.0045(5)
O6 0.0426(11) 0.0634(15) 0.0578(14) 0.0070(12) -0.0007(10) -0.0009(10)
O12 0.0526(13) 0.0600(15) 0.0662(16) 0.0216(13) 0.0061(11) 0.0011(11)
O11 0.0520(13) 0.0684(17) 0.0669(17) 0.0248(14) 0.0067(12) 0.0044(12)
O7 0.0538(13) 0.0671(17) 0.0600(15) 0.0151(13) -0.0074(11) -0.0074(12)
O00A 0.0797(18) 0.0644(17) 0.0611(16) 0.0205(14) -0.0052(14) 0.0002(14)
O5 0.0628(16) 0.085(2) 0.085(2) 0.0025(18) 0.0084(15) 0.0202(15)
O8 0.0731(17) 0.0648(17) 0.0657(17) -0.0062(14) -0.0078(14) -0.0044(14)
O10 0.0524(14) 0.097(2) 0.079(2) 0.0288(18) -0.0029(13) 0.0011(15)
O00E 0.0480(14) 0.117(3) 0.0736(19) 0.0325(19) 0.0052(13) -0.0036(15)
O2 0.078(2) 0.083(2) 0.097(3) -0.018(2) 0.0048(18) 0.0154(17)
N1 0.0521(17) 0.065(2) 0.078(2) -0.0072(18) -0.0071(15) 0.0016(15)
N2 0.066(2) 0.062(2) 0.067(2) 0.0055(17) 0.0026(16) 0.0092(16)
O9 0.119(3) 0.094(3) 0.082(2) -0.029(2) -0.010(2) -0.017(2)
O1 0.0518(16) 0.099(3) 0.154(4) -0.053(3) -0.0147(19) 0.0033(17)
O14 0.091(2) 0.080(2) 0.130(4) 0.007(2) -0.017(2) -0.025(2)
O13 0.144(4) 0.091(3) 0.074(2) 0.010(2) -0.029(2) -0.003(3)
O4 0.098(3) 0.141(4) 0.074(2) -0.007(2) 0.000(2) 0.010(3)
C24 0.0491(17) 0.055(2) 0.0530(19) 0.0132(16) 0.0005(14) -0.0001(15)
O3 0.099(3) 0.078(2) 0.195(5) 0.016(3) 0.017(3) -0.011(2)
C25 0.0543(19) 0.061(2) 0.071(2) 0.022(2) 0.0049(17) 0.0066(16)
C23 0.0528(18) 0.054(2) 0.055(2) 0.0144(17) -0.0015(15) 0.0002(15)
C3 0.047(2) 0.083(3) 0.100(4) -0.008(3) -0.008(2) 0.001(2)
C26 0.0492(17) 0.067(2) 0.066(2) 0.021(2) 0.0075(16) 0.0037(16)
O16 0.133(4) 0.200(6) 0.086(3) -0.022(3) 0.021(3) -0.060(4)
O15 0.151(4) 0.071(2) 0.170(4) -0.021(3) -0.004(3) 0.011(3)
C1 0.051(2) 0.078(3) 0.085(3) 0.004(2) -0.002(2) 0.007(2)
C30 0.074(3) 0.135(5) 0.093(4) 0.049(4) -0.021(3) -0.005(3)
C4 0.056(3) 0.146(7) 0.211(9) -0.075(6) -0.023(4) -0.004(3)
C36 0.072(3) 0.150(6) 0.083(4) 0.057(4) 0.004(3) -0.008(3)
C2 0.064(3) 0.119(5) 0.132(5) -0.018(4) -0.006(3) 0.024(3)
C17 0.190(8) 0.106(5) 0.077(4) 0.015(4) -0.040(5) -0.008(5)
C14 0.087(4) 0.099(5) 0.169(7) 0.018(5) 0.012(4) -0.013(3)
C20 0.226(10) 0.145(7) 0.089(5) 0.058(5) -0.012(6) 0.064(7)
C33 0.135(5) 0.119(5) 0.137(5) 0.013(4) 0.025(4) 0.068(4)
C31 0.139(7) 0.174(9) 0.140(7) 0.008(6) -0.061(6) -0.011(6)
C18 0.169(9) 0.167(9) 0.118(6) 0.015(6) -0.003(6) -0.037(7)
C11 0.188(6) 0.143(6) 0.127(5) -0.069(5) -0.011(5) -0.033(5)
C5 0.146(8) 0.263(16) 0.149(9) 0.044(10) 0.050(7) -0.028(9)
C38 0.179(9) 0.274(14) 0.080(5) 0.044(7) 0.029(5) 0.036(9)
C34 0.137(6) 0.098(5) 0.197(9) 0.048(5) 0.013(6) 0.040(5)
C15 0.125(6) 0.141(7) 0.163(8) 0.053(6) -0.005(6) 0.016(5)
C19 0.259(13) 0.173(10) 0.097(5) 0.031(6) -0.084(7) 0.006(9)
C28 0.159(6) 0.104(5) 0.259(8) 0.002(6) 0.060(6) -0.029(5)
C16 0.138(7) 0.141(8) 0.288(15) 0.056(9) -0.032(8) -0.078(6)
C32 0.186(9) 0.202(11) 0.177(10) 0.040(8) -0.076(8) 0.085(9)
C39 0.173(9) 0.39(2) 0.090(6) -0.084(9) -0.026(6) 0.017(12)
C6 0.213(13) 0.202(13) 0.160(10) 0.016(9) 0.036(9) -0.045(10)
C22 0.37(2) 0.316(18) 0.073(5) 0.013(8) -0.035(8) 0.191(16)
C37 0.292(15) 0.130(8) 0.146(8) 0.077(7) -0.079(9) -0.035(9)
C21 0.38(2) 0.182(11) 0.181(11) 0.075(9) -0.028(12) 0.161(13)
C8 0.219(8) 0.108(5) 0.245(8) -0.009(6) 0.044(7) 0.038(5)
C7 0.188(13) 0.239(17) 0.31(2) 0.079(16) 0.086(14) -0.009(12)
C41 0.228(16) 0.42(3) 0.224(17) -0.024(18) -0.113(14) 0.039(18)
C40 0.33(2) 0.32(2) 0.108(7) -0.040(10) 0.072(10) -0.037(16)
C29 0.270(13) 0.143(9) 0.359(16) -0.017(11) 0.087(12) -0.073(9)
C12 0.271(13) 0.293(13) 0.154(9) -0.115(9) 0.032(9) -0.099(11)
C35 0.297(12) 0.199(10) 0.248(11) 0.021(9) 0.139(10) 0.122(10)
C13 0.317(14) 0.182(11) 0.229(12) -0.073(10) -0.069(11) -0.067(11)
C9 0.324(15) 0.180(11) 0.313(15) -0.021(11) 0.080(13) 0.087(11)
C27 0.232(12) 0.215(12) 0.311(15) 0.033(11) 0.113(10) -0.007(10)
C10 0.311(15) 0.198(12) 0.355(16) 0.080(13) 0.116(14) 0.029(10)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2191 1.8069 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O00A Ti3 O6 95.85(14) . .
O00A Ti3 O8 97.09(15) . .
O6 Ti3 O8 145.85(12) . .
O00A Ti3 O12 167.10(13) . .
O6 Ti3 O12 87.62(12) . .
O8 Ti3 O12 86.73(13) . .
O00A Ti3 O7 104.99(13) . .
O6 Ti3 O7 74.43(11) . .
O8 Ti3 O7 71.73(13) . .
O12 Ti3 O7 87.90(11) . .
O00A Ti3 N1 90.23(15) . .
O6 Ti3 N1 73.53(12) . .
O8 Ti3 N1 137.68(13) . .
O12 Ti3 N1 78.81(13) . .
O7 Ti3 N1 145.67(13) . .
O00A Ti3 N2 85.65(14) . .
O6 Ti3 N2 141.05(13) . .
O8 Ti3 N2 71.54(14) . .
O12 Ti3 N2 83.88(12) . .
O7 Ti3 N2 142.72(14) . .
N1 Ti3 N2 67.54(14) . .
O00A Ti3 Ti2 108.78(11) . .
O6 Ti3 Ti2 37.76(7) . .
O8 Ti3 Ti2 108.10(9) . .
O12 Ti3 Ti2 81.47(8) . .
O7 Ti3 Ti2 37.42(9) . .
N1 Ti3 Ti2 108.71(10) . .
N2 Ti3 Ti2 165.34(10) . .
O00A Ti3 Ti4 105.12(11) . .
O6 Ti3 Ti4 110.42(8) . .
O8 Ti3 Ti4 35.52(9) . .
O12 Ti3 Ti4 85.14(9) . .
O7 Ti3 Ti4 36.27(9) . .
N1 Ti3 Ti4 163.37(11) . .
N2 Ti3 Ti4 106.64(11) . .
Ti2 Ti3 Ti4 72.78(3) . .
O10 Ti2 O00E 96.94(14) . .
O10 Ti2 O7 105.69(15) . .
O00E Ti2 O7 99.30(16) . .
O10 Ti2 O6 166.61(13) . .
O00E Ti2 O6 95.51(12) . .
O7 Ti2 O6 76.99(11) . .
O10 Ti2 O5 100.69(16) . .
O00E Ti2 O5 94.98(17) . .
O7 Ti2 O5 148.07(12) . .
O6 Ti2 O5 73.30(12) . .
O10 Ti2 O11 85.01(12) . .
O00E Ti2 O11 175.80(16) . .
O7 Ti2 O11 83.70(12) . .
O6 Ti2 O11 82.25(11) . .
O5 Ti2 O11 80.98(13) . .
O10 Ti2 Ti3 141.84(13) . .
O00E Ti2 Ti3 105.32(11) . .
O7 Ti2 Ti3 40.93(8) . .
O6 Ti2 Ti3 36.85(8) . .
O5 Ti2 Ti3 107.65(9) . .
O11 Ti2 Ti3 75.00(7) . .
O10 Ti2 Ti1 137.03(13) . .
O00E Ti2 Ti1 98.33(12) . .
O7 Ti2 Ti1 111.04(8) . .
O6 Ti2 Ti1 35.22(8) . .
O5 Ti2 Ti1 38.16(8) . .
O11 Ti2 Ti1 77.78(8) . .
Ti3 Ti2 Ti1 70.12(2) . .
O4 Ti1 O3 107.1(3) . .
O4 Ti1 O6 112.23(19) . .
O3 Ti1 O6 140.5(2) . .
O4 Ti1 O1 100.5(2) . .
O3 Ti1 O1 89.1(2) . .
O6 Ti1 O1 81.10(13) . .
O4 Ti1 O5 103.85(17) . .
O3 Ti1 O5 96.8(2) . .
O6 Ti1 O5 76.95(13) . .
O1 Ti1 O5 151.93(17) . .
O4 Ti1 Ti2 115.30(16) . .
O3 Ti1 Ti2 124.2(2) . .
O6 Ti1 Ti2 36.92(7) . .
O1 Ti1 Ti2 115.54(11) . .
O5 Ti1 Ti2 40.11(11) . .
O13 Ti4 O14 108.2(2) . .
O13 Ti4 O8 124.4(2) . .
O14 Ti4 O8 126.50(17) . .
O13 Ti4 O7 103.31(17) . .
O14 Ti4 O7 100.25(18) . .
O8 Ti4 O7 78.00(13) . .
O13 Ti4 O9 96.0(2) . .
O14 Ti4 O9 95.1(2) . .
O8 Ti4 O9 72.16(15) . .
O7 Ti4 O9 150.01(15) . .
O13 Ti4 Ti3 119.58(15) . .
O14 Ti4 Ti3 121.97(16) . .
O8 Ti4 Ti3 37.55(9) . .
O7 Ti4 Ti3 40.52(8) . .
O9 Ti4 Ti3 109.71(12) . .
O13 Ti4 Ti5 114.27(18) . .
O14 Ti4 Ti5 117.31(15) . .
O8 Ti4 Ti5 33.73(10) . .
O7 Ti4 Ti5 111.73(9) . .
O9 Ti4 Ti5 38.47(12) . .
Ti3 Ti4 Ti5 71.26(3) . .
O15 Ti5 O16 111.6(3) . .
O15 Ti5 O8 126.4(2) . .
O16 Ti5 O8 121.9(3) . .
O15 Ti5 O2 94.0(2) . .
O16 Ti5 O2 94.3(2) . .
O8 Ti5 O2 80.85(14) . .
O15 Ti5 O9 99.8(2) . .
O16 Ti5 O9 100.3(2) . .
O8 Ti5 O9 73.74(15) . .
O2 Ti5 O9 154.54(16) . .
O15 Ti5 Ti4 121.0(2) . .
O16 Ti5 Ti4 115.9(2) . .
O8 Ti5 Ti4 33.81(9) . .
O2 Ti5 Ti4 114.65(11) . .
O9 Ti5 Ti4 39.98(12) . .
Ti1 O6 Ti3 138.65(13) . .
Ti1 O6 Ti2 107.86(13) . .
Ti3 O6 Ti2 105.39(13) . .
C23 O12 Ti3 128.1(2) . .
C23 O11 Ti2 130.1(2) . .
Ti4 O7 Ti2 150.12(15) . .
Ti4 O7 Ti3 103.21(14) . .
Ti2 O7 Ti3 101.65(13) . .
C20 O00A Ti3 159.5(6) . .
C33 O5 Ti1 127.7(5) . .
C33 O5 Ti2 130.0(5) . .
Ti1 O5 Ti2 101.73(14) . .
Ti5 O8 Ti4 112.47(15) . .
Ti5 O8 Ti3 140.55(17) . .
Ti4 O8 Ti3 106.93(15) . .
C30 O10 Ti2 150.7(3) . .
C36 O00E Ti2 134.4(3) . .
N2 O2 Ti5 121.2(3) . .
C3 N1 O1 116.9(4) . .
C3 N1 Ti3 121.7(3) . .
O1 N1 Ti3 121.3(2) . .
C1 N2 O2 115.7(4) . .
C1 N2 Ti3 121.5(3) . .
O2 N2 Ti3 121.7(3) . .
C11 O9 Ti5 134.1(5) . .
C11 O9 Ti4 124.4(5) . .
Ti5 O9 Ti4 101.55(16) . .
N1 O1 Ti1 123.5(3) . .
C14 O14 Ti4 141.9(4) . .
C17 O13 Ti4 149.3(5) . .
C39 O4 Ti1 149.1(8) . .
C25 C24 C26 118.9(4) . 3_666
C25 C24 C23 120.8(3) . .
C26 C24 C23 120.2(3) 3_666 .
C28 O3 Ti1 149.8(5) . .
C26 C25 C24 120.6(4) . .
C26 C25 H25 119.7 . .
C24 C25 H25 119.7 . .
O11 C23 O12 125.3(3) . .
O11 C23 C24 118.9(3) . .
O12 C23 C24 115.8(3) . .
N1 C3 C1 114.5(4) . .
N1 C3 C4 122.2(5) . .
C1 C3 C4 123.3(4) . .
C25 C26 C24 120.5(4) . 3_666
C25 C26 H26 119.8 . .
C24 C26 H26 119.8 3_666 .
C5 O16 Ti5 143.7(7) . .
C8 O15 Ti5 149.8(7) . .
N2 C1 C3 114.1(4) . .
N2 C1 C2 123.4(5) . .
C3 C1 C2 122.4(5) . .
O10 C30 C31 110.8(6) . .
O10 C30 C32 110.3(6) . .
C31 C30 C32 108.3(7) . .
O10 C30 H30 109.1 . .
C31 C30 H30 109.1 . .
C32 C30 H30 109.1 . .
C3 C4 H4A 109.5 . .
C3 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
C3 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
O00E C36 C37 108.6(6) . .
O00E C36 C38 108.1(6) . .
C37 C36 C38 117.1(8) . .
O00E C36 H36 107.5 . .
C37 C36 H36 107.5 . .
C38 C36 H36 107.5 . .
C1 C2 H2A 109.5 . .
C1 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
C1 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
O13 C17 C18 108.4(7) . .
O13 C17 C19 107.7(7) . .
C18 C17 C19 113.9(8) . .
O13 C17 H17 108.9 . .
C18 C17 H17 108.9 . .
C19 C17 H17 108.9 . .
O14 C14 C16 110.8(8) . .
O14 C14 C15 110.2(6) . .
C16 C14 C15 113.0(8) . .
O14 C14 H14 107.5 . .
C16 C14 H14 107.5 . .
C15 C14 H14 107.5 . .
C21 C20 O00A 114.4(8) . .
C21 C20 C22 127.4(9) . .
O00A C20 C22 114.5(8) . .
C21 C20 H20 96.4 . .
O00A C20 H20 96.4 . .
C22 C20 H20 96.4 . .
C35 C33 O5 110.7(7) . .
C35 C33 C34 133.0(8) . .
O5 C33 C34 115.2(6) . .
C35 C33 H33 93.5 . .
O5 C33 H33 93.5 . .
C34 C33 H33 93.5 . .
C30 C31 H31A 109.5 . .
C30 C31 H31B 109.5 . .
H31A C31 H31B 109.5 . .
C30 C31 H31C 109.5 . .
H31A C31 H31C 109.5 . .
H31B C31 H31C 109.5 . .
C17 C18 H18A 109.5 . .
C17 C18 H18B 109.5 . .
H18A C18 H18B 109.5 . .
C17 C18 H18C 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
O9 C11 C12 108.1(8) . .
O9 C11 C13 109.7(9) . .
C12 C11 C13 111.2(11) . .
O9 C11 H11 109.2 . .
C12 C11 H11 109.2 . .
C13 C11 H11 109.2 . .
C6 C5 O16 117.8(12) . .
C6 C5 C7 116.4(11) . .
O16 C5 C7 106.0(12) . .
C6 C5 H5 105.1 . .
O16 C5 H5 105.1 . .
C7 C5 H5 105.1 . .
C36 C38 H38A 109.5 . .
C36 C38 H38B 109.5 . .
H38A C38 H38B 109.5 . .
C36 C38 H38C 109.5 . .
H38A C38 H38C 109.5 . .
H38B C38 H38C 109.5 . .
C33 C34 H34A 109.5 . .
C33 C34 H34B 109.5 . .
H34A C34 H34B 109.5 . .
C33 C34 H34C 109.5 . .
H34A C34 H34C 109.5 . .
H34B C34 H34C 109.5 . .
C14 C15 H15A 109.5 . .
C14 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
C14 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
C17 C19 H19A 109.5 . .
C17 C19 H19B 109.5 . .
H19A C19 H19B 109.5 . .
C17 C19 H19C 109.5 . .
H19A C19 H19C 109.5 . .
H19B C19 H19C 109.5 . .
O3 C28 C27 119.6(9) . .
O3 C28 C29 110.4(9) . .
C27 C28 C29 129.9(11) . .
O3 C28 H28 90.7 . .
C27 C28 H28 90.7 . .
C29 C28 H28 90.7 . .
C14 C16 H16A 109.5 . .
C14 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
C14 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
C30 C32 H32A 109.5 . .
C30 C32 H32B 109.5 . .
H32A C32 H32B 109.5 . .
C30 C32 H32C 109.5 . .
H32A C32 H32C 109.5 . .
H32B C32 H32C 109.5 . .
O4 C39 C41 118.2(12) . .
O4 C39 C40 117.6(11) . .
C41 C39 C40 122.7(12) . .
C5 C6 H6A 109.5 . .
C5 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
C5 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
C20 C22 H22A 109.5 . .
C20 C22 H22B 109.5 . .
H22A C22 H22B 109.5 . .
C20 C22 H22C 109.5 . .
H22A C22 H22C 109.5 . .
H22B C22 H22C 109.5 . .
C36 C37 H37A 109.5 . .
C36 C37 H37B 109.5 . .
H37A C37 H37B 109.5 . .
C36 C37 H37C 109.5 . .
H37A C37 H37C 109.5 . .
H37B C37 H37C 109.5 . .
C20 C21 H21A 109.5 . .
C20 C21 H21B 109.5 . .
H21A C21 H21B 109.5 . .
C20 C21 H21C 109.5 . .
H21A C21 H21C 109.5 . .
H21B C21 H21C 109.5 . .
C9 C8 O15 106.9(13) . .
C9 C8 C10 97.1(12) . .
O15 C8 C10 106.3(12) . .
C9 C8 H8 114.9 . .
O15 C8 H8 114.9 . .
C10 C8 H8 114.9 . .
C5 C7 H7A 109.5 . .
C5 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C5 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
C39 C41 H41A 109.5 . .
C39 C41 H41B 109.5 . .
H41A C41 H41B 109.5 . .
C39 C41 H41C 109.5 . .
H41A C41 H41C 109.5 . .
H41B C41 H41C 109.5 . .
C39 C40 H40A 109.5 . .
C39 C40 H40B 109.5 . .
H40A C40 H40B 109.5 . .
C39 C40 H40C 109.5 . .
H40A C40 H40C 109.5 . .
H40B C40 H40C 109.5 . .
C28 C29 H29A 109.5 . .
C28 C29 H29B 109.5 . .
H29A C29 H29B 109.5 . .
C28 C29 H29C 109.5 . .
H29A C29 H29C 109.5 . .
H29B C29 H29C 109.5 . .
C11 C12 H12A 109.5 . .
C11 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C11 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
C33 C35 H35A 109.5 . .
C33 C35 H35B 109.5 . .
H35A C35 H35B 109.5 . .
C33 C35 H35C 109.5 . .
H35A C35 H35C 109.5 . .
H35B C35 H35C 109.5 . .
C11 C13 H13A 109.5 . .
C11 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
C11 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
C8 C9 H9A 109.5 . .
C8 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
C8 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
C28 C27 H27A 109.5 . .
C28 C27 H27B 109.5 . .
H27A C27 H27B 109.5 . .
C28 C27 H27C 109.5 . .
H27A C27 H27C 109.5 . .
H27B C27 H27C 109.5 . .
C8 C10 H10A 109.5 . .
C8 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C8 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ti3 O00A 1.770(3) .
Ti3 O6 1.940(3) .
Ti3 O8 1.992(3) .
Ti3 O12 2.065(3) .
Ti3 O7 2.087(3) .
Ti3 N1 2.253(4) .
Ti3 N2 2.262(4) .
Ti3 Ti2 3.1196(10) .
Ti3 Ti4 3.1266(11) .
Ti2 O10 1.796(3) .
Ti2 O00E 1.809(3) .
Ti2 O7 1.936(3) .
Ti2 O6 1.981(2) .
Ti2 O5 2.066(4) .
Ti2 O11 2.213(3) .
Ti2 Ti1 3.1392(11) .
Ti1 O4 1.765(4) .
Ti1 O3 1.776(4) .
Ti1 O6 1.902(3) .
Ti1 O1 1.951(3) .
Ti1 O5 1.981(3) .
Ti4 O13 1.787(4) .
Ti4 O14 1.794(4) .
Ti4 O8 1.899(3) .
Ti4 O7 1.900(3) .
Ti4 O9 2.068(4) .
Ti4 Ti5 3.1536(14) .
Ti5 O15 1.759(5) .
Ti5 O16 1.772(5) .
Ti5 O8 1.895(3) .
Ti5 O2 1.954(4) .
Ti5 O9 2.003(4) .
O12 C23 1.273(5) .
O11 C23 1.251(5) .
O00A C20 1.397(7) .
O5 C33 1.437(7) .
O10 C30 1.415(6) .
O00E C36 1.421(6) .
O2 N2 1.358(5) .
N1 C3 1.298(6) .
N1 O1 1.336(5) .
N2 C1 1.294(6) .
O9 C11 1.457(8) .
O14 C14 1.389(8) .
O13 C17 1.413(8) .
O4 C39 1.354(9) .
C24 C25 1.384(5) .
C24 C26 1.390(5) 3_666
C24 C23 1.497(5) .
O3 C28 1.410(10) .
C25 C26 1.378(5) .
C25 H25 0.9300 .
C3 C1 1.438(7) .
C3 C4 1.501(7) .
C26 C24 1.390(5) 3_666
C26 H26 0.9300 .
O16 C5 1.424(11) .
O15 C8 1.456(13) .
C1 C2 1.509(6) .
C30 C31 1.472(11) .
C30 C32 1.510(12) .
C30 H30 0.9800 .
C4 H4A 0.9600 .
C4 H4B 0.9600 .
C4 H4C 0.9600 .
C36 C37 1.463(11) .
C36 C38 1.537(12) .
C36 H36 0.9800 .
C2 H2A 0.9600 .
C2 H2B 0.9600 .
C2 H2C 0.9600 .
C17 C18 1.514(13) .
C17 C19 1.516(11) .
C17 H17 0.9800 .
C14 C16 1.474(11) .
C14 C15 1.501(10) .
C14 H14 0.9800 .
C20 C21 1.400(13) .
C20 C22 1.410(14) .
C20 H20 0.9800 .
C33 C35 1.437(8) .
C33 C34 1.441(11) .
C33 H33 0.9800 .
C31 H31A 0.9600 .
C31 H31B 0.9600 .
C31 H31C 0.9600 .
C18 H18A 0.9600 .
C18 H18B 0.9600 .
C18 H18C 0.9600 .
C11 C12 1.461(8) .
C11 C13 1.513(16) .
C11 H11 0.9800 .
C5 C6 1.363(16) .
C5 C7 1.458(17) .
C5 H5 0.9800 .
C38 H38A 0.9600 .
C38 H38B 0.9600 .
C38 H38C 0.9600 .
C34 H34A 0.9600 .
C34 H34B 0.9600 .
C34 H34C 0.9600 .
C15 H15A 0.9600 .
C15 H15B 0.9600 .
C15 H15C 0.9600 .
C19 H19A 0.9600 .
C19 H19B 0.9600 .
C19 H19C 0.9600 .
C28 C27 1.453(9) .
C28 C29 1.467(8) .
C28 H28 0.9800 .
C16 H16A 0.9600 .
C16 H16B 0.9600 .
C16 H16C 0.9600 .
C32 H32A 0.9600 .
C32 H32B 0.9600 .
C32 H32C 0.9600 .
C39 C41 1.355(17) .
C39 C40 1.434(16) .
C6 H6A 0.9600 .
C6 H6B 0.9600 .
C6 H6C 0.9600 .
C22 H22A 0.9600 .
C22 H22B 0.9600 .
C22 H22C 0.9600 .
C37 H37A 0.9600 .
C37 H37B 0.9600 .
C37 H37C 0.9600 .
C21 H21A 0.9600 .
C21 H21B 0.9600 .
C21 H21C 0.9600 .
C8 C9 1.387(17) .
C8 C10 1.483(9) .
C8 H8 0.9800 .
C7 H7A 0.9600 .
C7 H7B 0.9600 .
C7 H7C 0.9600 .
C41 H41A 0.9600 .
C41 H41B 0.9600 .
C41 H41C 0.9600 .
C40 H40A 0.9600 .
C40 H40B 0.9600 .
C40 H40C 0.9600 .
C29 H29A 0.9600 .
C29 H29B 0.9600 .
C29 H29C 0.9600 .
C12 H12A 0.9600 .
C12 H12B 0.9600 .
C12 H12C 0.9600 .
C35 H35A 0.9600 .
C35 H35B 0.9600 .
C35 H35C 0.9600 .
C13 H13A 0.9600 .
C13 H13B 0.9600 .
C13 H13C 0.9600 .
C9 H9A 0.9600 .
C9 H9B 0.9600 .
C9 H9C 0.9600 .
C27 H27A 0.9600 .
C27 H27B 0.9600 .
C27 H27C 0.9600 .
C10 H10A 0.9600 .
C10 H10B 0.9600 .
C10 H10C 0.9600 .