#------------------------------------------------------------------------------
#$Date: 2016-03-25 09:41:49 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179731 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/27/7002776.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_7002776
loop_
_publ_author_name
'Crimmin, Mark R.'
'Barrett, Anthony G. M.'
'Hill, Michael S.'
'MacDougall, Dugald J.'
'Mahon, Mary F.'
'Procopiou, Panayiotis A.'
_publ_section_title
;
 β-Diketiminate C--H activation with heavier group 2 alkyls
;
_journal_issue                   44
_journal_name_full               'Dalton Transactions'
_journal_page_first              9715
_journal_page_last               9717
_journal_paper_doi               10.1039/b917466b
_journal_year                    2009
_chemical_formula_sum            'C42 H61 Ca N3 O'
_chemical_formula_weight         664.02
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.125(1)
_cell_angle_beta                 91.025(1)
_cell_angle_gamma                97.899(1)
_cell_formula_units_Z            4
_cell_length_a                   12.2139(2)
_cell_length_b                   17.7982(4)
_cell_length_c                   18.2010(5)
_cell_measurement_reflns_used    54565
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      2.910
_cell_volume                     3918.42(15)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'Denzo & Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEX (P.McArdle, 1995)'
_computing_publication_material  'SHELXL-97/2 (Sheldrick,1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  '95mm CCD camera on κ-goniostat'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1176
_diffrn_reflns_av_sigmaI/netI    0.0878
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            65141
_diffrn_reflns_theta_full        25.07
_diffrn_reflns_theta_max         25.07
_diffrn_reflns_theta_min         3.84
_exptl_absorpt_coefficient_mu    0.194
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.88
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.126
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.474
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     844
_refine_ls_number_reflns         13817
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.1253
_refine_ls_R_factor_gt           0.0654
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0346P)²+5.2857P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1286
_refine_ls_wR_factor_ref         0.1575
_reflns_number_gt                8509
_reflns_number_total             13817
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b917466b.txt
_cod_data_source_block
c:\x-ray\kappa\old_ka~1\k08msh~1\maxus2\k08msh57
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-Scan' changed
to 'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7002776
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C -0.2898(4) -0.7890(2) 0.7365(3) 0.0534(12) Uani 1 1 d . . .
H1A H -0.3601 -0.7931 0.7634 0.064 Uiso 1 1 calc R . .
H1B H -0.2362 -0.7463 0.7556 0.064 Uiso 1 1 calc R . .
C2 C -0.3037(3) -0.7892(2) 0.6588(2) 0.0422(10) Uani 1 1 d . . .
C3 C -0.2163(3) -0.7968(2) 0.6100(2) 0.0355(9) Uani 1 1 d . . .
C4 C -0.2336(4) -0.7990(2) 0.5338(2) 0.0483(11) Uani 1 1 d . . .
H4 H -0.1727 -0.8019 0.5027 0.058 Uiso 1 1 calc R . .
C5 C -0.3366(5) -0.7972(3) 0.5029(3) 0.0663(15) Uani 1 1 d . . .
H5 H -0.3474 -0.7994 0.4510 0.080 Uiso 1 1 calc R . .
C6 C -0.4241(5) -0.7922(3) 0.5489(4) 0.0715(17) Uani 1 1 d . . .
H6 H -0.4959 -0.7913 0.5283 0.086 Uiso 1 1 calc R . .
C7 C -0.4094(4) -0.7883(2) 0.6237(3) 0.0600(14) Uani 1 1 d . . .
H7 H -0.4717 -0.7849 0.6534 0.072 Uiso 1 1 calc R . .
C8 C -0.0341(3) -0.8372(3) 0.5949(2) 0.0526(12) Uani 1 1 d . . .
H8A H 0.0365 -0.8390 0.6207 0.079 Uiso 1 1 calc R . .
H8B H -0.0216 -0.8069 0.5501 0.079 Uiso 1 1 calc R . .
H8C H -0.0676 -0.8888 0.5818 0.079 Uiso 1 1 calc R . .
C9 C -0.0526(3) -0.7274(2) 0.6653(3) 0.0554(12) Uani 1 1 d . . .
H9A H 0.0197 -0.7326 0.6874 0.083 Uiso 1 1 calc R . .
H9B H -0.0976 -0.7051 0.7014 0.083 Uiso 1 1 calc R . .
H9C H -0.0427 -0.6944 0.6223 0.083 Uiso 1 1 calc R . .
C10 C -0.2810(3) -1.0416(2) 0.8606(2) 0.0351(9) Uani 1 1 d . . .
C11 C -0.1829(3) -1.0734(2) 0.8529(2) 0.0361(9) Uani 1 1 d . . .
H11 H -0.1840 -1.1229 0.8725 0.043 Uiso 1 1 calc R . .
C12 C -0.0834(3) -1.0429(2) 0.8206(2) 0.0311(8) Uani 1 1 d . . .
C13 C 0.0149(3) -1.0837(2) 0.8392(2) 0.0417(10) Uani 1 1 d . . .
H13A H 0.0806 -1.0587 0.8144 0.063 Uiso 1 1 calc R . .
H13B H -0.0008 -1.1366 0.8227 0.063 Uiso 1 1 calc R . .
H13C H 0.0283 -1.0822 0.8925 0.063 Uiso 1 1 calc R . .
C14 C -0.3639(3) -1.0826(2) 0.9132(2) 0.0513(11) Uani 1 1 d . . .
H14A H -0.3805 -1.0473 0.9515 0.077 Uiso 1 1 calc R . .
H14B H -0.3327 -1.1250 0.9359 0.077 Uiso 1 1 calc R . .
H14C H -0.4321 -1.1020 0.8861 0.077 Uiso 1 1 calc R . .
C15 C 0.0340(3) -0.9509(2) 0.7513(2) 0.0304(8) Uani 1 1 d . . .
C16 C 0.0828(3) -0.9843(2) 0.6924(2) 0.0320(8) Uani 1 1 d . . .
C17 C 0.1774(3) -0.9445(2) 0.6619(2) 0.0395(9) Uani 1 1 d . . .
H17 H 0.2110 -0.9663 0.6219 0.047 Uiso 1 1 calc R . .
C18 C 0.2234(3) -0.8745(2) 0.6883(2) 0.0436(10) Uani 1 1 d . . .
H18 H 0.2862 -0.8476 0.6653 0.052 Uiso 1 1 calc R . .
C19 C 0.1781(3) -0.8434(2) 0.7482(2) 0.0404(10) Uani 1 1 d . . .
H19 H 0.2119 -0.7960 0.7675 0.049 Uiso 1 1 calc R . .
C20 C 0.0836(3) -0.8804(2) 0.7807(2) 0.0335(9) Uani 1 1 d . . .
C21 C 0.0355(3) -1.0611(2) 0.6595(2) 0.0347(9) Uani 1 1 d . . .
H21 H -0.0299 -1.0821 0.6889 0.042 Uiso 1 1 calc R . .
C22 C 0.1186(3) -1.1182(2) 0.6620(2) 0.0464(10) Uani 1 1 d . . .
H22A H 0.0844 -1.1665 0.6405 0.070 Uiso 1 1 calc R . .
H22B H 0.1405 -1.1261 0.7131 0.070 Uiso 1 1 calc R . .
H22C H 0.1840 -1.0985 0.6339 0.070 Uiso 1 1 calc R . .
C23 C -0.0041(3) -1.0526(2) 0.5802(2) 0.0431(10) Uani 1 1 d . . .
H23A H -0.0344 -1.1025 0.5604 0.065 Uiso 1 1 calc R . .
H23B H 0.0583 -1.0307 0.5504 0.065 Uiso 1 1 calc R . .
H23C H -0.0615 -1.0192 0.5789 0.065 Uiso 1 1 calc R . .
C24 C 0.0371(3) -0.8475(2) 0.8496(2) 0.0420(10) Uani 1 1 d . . .
H24 H -0.0453 -0.8550 0.8439 0.050 Uiso 1 1 calc R . .
C25 C 0.0653(4) -0.8904(3) 0.9179(2) 0.0575(12) Uani 1 1 d . . .
H25A H 0.0408 -0.9447 0.9106 0.086 Uiso 1 1 calc R . .
H25B H 0.0277 -0.8722 0.9602 0.086 Uiso 1 1 calc R . .
H25C H 0.1454 -0.8818 0.9268 0.086 Uiso 1 1 calc R . .
C26 C 0.0737(4) -0.7631(2) 0.8606(3) 0.0607(13) Uani 1 1 d . . .
H26A H 0.0547 -0.7357 0.8165 0.091 Uiso 1 1 calc R . .
H26B H 0.1538 -0.7540 0.8693 0.091 Uiso 1 1 calc R . .
H26C H 0.0361 -0.7452 0.9030 0.091 Uiso 1 1 calc R . .
C27 C -0.3964(3) -0.9452(2) 0.8517(2) 0.0317(8) Uani 1 1 d . . .
C28 C -0.3826(3) -0.8923(2) 0.9100(2) 0.0350(9) Uani 1 1 d . . .
C29 C -0.4707(3) -0.8546(2) 0.9282(2) 0.0421(10) Uani 1 1 d . . .
H29 H -0.4616 -0.8183 0.9669 0.050 Uiso 1 1 calc R . .
C30 C -0.5715(3) -0.8687(2) 0.8912(2) 0.0448(10) Uani 1 1 d . . .
H30 H -0.6306 -0.8420 0.9039 0.054 Uiso 1 1 calc R . .
C31 C -0.5848(3) -0.9219(2) 0.8357(2) 0.0452(10) Uani 1 1 d . . .
H31 H -0.6543 -0.9323 0.8108 0.054 Uiso 1 1 calc R . .
C32 C -0.4992(3) -0.9608(2) 0.8152(2) 0.0382(9) Uani 1 1 d . . .
C33 C -0.5170(3) -1.0175(2) 0.7515(2) 0.0449(10) Uani 1 1 d . . .
H33 H -0.4487 -1.0424 0.7476 0.054 Uiso 1 1 calc R . .
C34 C -0.5342(4) -0.9783(3) 0.6791(2) 0.0556(12) Uani 1 1 d . . .
H34A H -0.5446 -1.0160 0.6394 0.083 Uiso 1 1 calc R . .
H34B H -0.4693 -0.9411 0.6693 0.083 Uiso 1 1 calc R . .
H34C H -0.5999 -0.9524 0.6820 0.083 Uiso 1 1 calc R . .
C35 C -0.6139(4) -1.0794(3) 0.7657(3) 0.0656(14) Uani 1 1 d . . .
H35A H -0.6228 -1.1152 0.7244 0.098 Uiso 1 1 calc R . .
H35B H -0.6817 -1.0563 0.7710 0.098 Uiso 1 1 calc R . .
H35C H -0.5993 -1.1064 0.8109 0.098 Uiso 1 1 calc R . .
C36 C -0.2742(3) -0.8761(2) 0.9533(2) 0.0438(10) Uani 1 1 d . . .
H36 H -0.2214 -0.9086 0.9328 0.053 Uiso 1 1 calc R . .
C37 C -0.2905(5) -0.8962(4) 1.0350(3) 0.0842(18) Uani 1 1 d . . .
H37A H -0.3234 -0.9494 1.0393 0.126 Uiso 1 1 calc R . .
H37B H -0.3398 -0.8635 1.0568 0.126 Uiso 1 1 calc R . .
H37C H -0.2188 -0.8885 1.0609 0.126 Uiso 1 1 calc R . .
C38 C -0.2230(4) -0.7942(3) 0.9473(3) 0.0587(12) Uani 1 1 d . . .
H38A H -0.1533 -0.7863 0.9756 0.088 Uiso 1 1 calc R . .
H38B H -0.2739 -0.7614 0.9669 0.088 Uiso 1 1 calc R . .
H38C H -0.2087 -0.7819 0.8956 0.088 Uiso 1 1 calc R . .
C39 C -0.2783(3) -1.0794(2) 0.6450(2) 0.0395(9) Uani 1 1 d . . .
H39A H -0.2977 -1.0888 0.6971 0.047 Uiso 1 1 calc R . .
H39B H -0.2100 -1.1015 0.6348 0.047 Uiso 1 1 calc R . .
C40 C -0.3031(3) -0.9867(2) 0.5556(2) 0.0399(9) Uani 1 1 d . . .
H40A H -0.2418 -0.9639 0.5243 0.048 Uiso 1 1 calc R . .
H40B H -0.3608 -0.9527 0.5561 0.048 Uiso 1 1 calc R . .
C41 C -0.3504(4) -1.0648(3) 0.5272(2) 0.0625(14) Uani 1 1 d . . .
H41A H -0.2977 -1.0853 0.4945 0.075 Uiso 1 1 calc R . .
H41B H -0.4208 -1.0630 0.4998 0.075 Uiso 1 1 calc R . .
C42 C -0.3694(4) -1.1128(2) 0.5959(3) 0.0547(12) Uani 1 1 d . . .
H42A H -0.4423 -1.1084 0.6173 0.066 Uiso 1 1 calc R . .
H42B H -0.3647 -1.1668 0.5854 0.066 Uiso 1 1 calc R . .
C43 C -0.1836(4) -0.2732(2) 0.7210(2) 0.0507(11) Uani 1 1 d . . .
H43A H -0.2136 -0.2387 0.7557 0.061 Uiso 1 1 calc R . .
H43B H -0.1019 -0.2637 0.7200 0.061 Uiso 1 1 calc R . .
C44 C -0.2360(3) -0.2783(2) 0.6506(2) 0.0373(9) Uani 1 1 d . . .
C45 C -0.3505(3) -0.3052(2) 0.6382(2) 0.0311(8) Uani 1 1 d . . .
C46 C -0.3963(3) -0.3129(2) 0.5678(2) 0.0357(9) Uani 1 1 d . . .
H46 H -0.4734 -0.3289 0.5618 0.043 Uiso 1 1 calc R . .
C47 C -0.3321(4) -0.2978(2) 0.5062(2) 0.0480(11) Uani 1 1 d . . .
H47 H -0.3642 -0.3039 0.4583 0.058 Uiso 1 1 calc R . .
C48 C -0.2214(4) -0.2741(3) 0.5158(3) 0.0524(12) Uani 1 1 d . . .
H48 H -0.1763 -0.2642 0.4740 0.063 Uiso 1 1 calc R . .
C49 C -0.1743(3) -0.2645(2) 0.5846(3) 0.0502(11) Uani 1 1 d . . .
H49 H -0.0972 -0.2479 0.5888 0.060 Uiso 1 1 calc R . .
C50 C -0.5219(3) -0.3728(3) 0.6880(3) 0.0567(12) Uani 1 1 d . . .
H50A H -0.5614 -0.3832 0.7341 0.085 Uiso 1 1 calc R . .
H50B H -0.5074 -0.4207 0.6660 0.085 Uiso 1 1 calc R . .
H50C H -0.5671 -0.3470 0.6539 0.085 Uiso 1 1 calc R . .
C51 C -0.4408(4) -0.2558(3) 0.7420(2) 0.0617(14) Uani 1 1 d . . .
H51A H -0.4852 -0.2709 0.7852 0.093 Uiso 1 1 calc R . .
H51B H -0.4820 -0.2260 0.7090 0.093 Uiso 1 1 calc R . .
H51C H -0.3714 -0.2252 0.7576 0.093 Uiso 1 1 calc R . .
C52 C -0.0970(3) -0.5231(2) 0.81553(19) 0.0306(8) Uani 1 1 d . . .
C53 C -0.1875(3) -0.5702(2) 0.8426(2) 0.0339(9) Uani 1 1 d . . .
H53 H -0.1733 -0.6195 0.8559 0.041 Uiso 1 1 calc R . .
C54 C -0.2975(3) -0.5563(2) 0.8534(2) 0.0321(8) Uani 1 1 d . . .
C55 C -0.3635(3) -0.6131(2) 0.9043(2) 0.0435(10) Uani 1 1 d . . .
H55A H -0.4384 -0.6000 0.9092 0.065 Uiso 1 1 calc R . .
H55B H -0.3270 -0.6114 0.9528 0.065 Uiso 1 1 calc R . .
H55C H -0.3676 -0.6643 0.8836 0.065 Uiso 1 1 calc R . .
C56 C 0.0147(3) -0.5508(2) 0.8275(2) 0.0410(10) Uani 1 1 d . . .
H56A H 0.0543 -0.5485 0.7810 0.062 Uiso 1 1 calc R . .
H56B H 0.0033 -0.6032 0.8451 0.062 Uiso 1 1 calc R . .
H56C H 0.0583 -0.5184 0.8641 0.062 Uiso 1 1 calc R . .
C57 C -0.0007(3) -0.4056(2) 0.7755(2) 0.0332(9) Uani 1 1 d . . .
C58 C 0.0613(3) -0.4032(2) 0.7107(2) 0.0402(10) Uani 1 1 d . . .
C59 C 0.1543(3) -0.3489(3) 0.7055(3) 0.0555(12) Uani 1 1 d . . .
H59 H 0.1961 -0.3463 0.6618 0.067 Uiso 1 1 calc R . .
C60 C 0.1874(3) -0.2987(3) 0.7619(3) 0.0555(12) Uani 1 1 d . . .
H60 H 0.2510 -0.2620 0.7571 0.067 Uiso 1 1 calc R . .
C61 C 0.1276(3) -0.3024(2) 0.8251(2) 0.0469(11) Uani 1 1 d . . .
H61 H 0.1518 -0.2684 0.8643 0.056 Uiso 1 1 calc R . .
C62 C 0.0329(3) -0.3543(2) 0.8337(2) 0.0371(9) Uani 1 1 d . . .
C63 C 0.0286(3) -0.4584(3) 0.6477(2) 0.0524(12) Uani 1 1 d . . .
H63 H -0.0386 -0.4931 0.6626 0.063 Uiso 1 1 calc R . .
C64 C 0.1186(4) -0.5073(3) 0.6302(3) 0.0713(15) Uani 1 1 d . . .
H64A H 0.0932 -0.5421 0.5898 0.107 Uiso 1 1 calc R . .
H64B H 0.1345 -0.5364 0.6738 0.107 Uiso 1 1 calc R . .
H64C H 0.1859 -0.4745 0.6158 0.107 Uiso 1 1 calc R . .
C65 C -0.0020(5) -0.4162(3) 0.5796(3) 0.0762(16) Uani 1 1 d . . .
H65A H -0.0234 -0.4525 0.5397 0.114 Uiso 1 1 calc R . .
H65B H 0.0616 -0.3801 0.5648 0.114 Uiso 1 1 calc R . .
H65C H -0.0641 -0.3886 0.5905 0.114 Uiso 1 1 calc R . .
C66 C -0.0315(4) -0.3566(2) 0.9043(2) 0.0452(10) Uani 1 1 d . . .
H66 H -0.1005 -0.3933 0.8972 0.054 Uiso 1 1 calc R . .
C67 C 0.0341(5) -0.3840(3) 0.9692(3) 0.0724(15) Uani 1 1 d . . .
H67A H -0.0101 -0.3850 1.0137 0.109 Uiso 1 1 calc R . .
H67B H 0.1030 -0.3493 0.9766 0.109 Uiso 1 1 calc R . .
H67C H 0.0512 -0.4351 0.9587 0.109 Uiso 1 1 calc R . .
C68 C -0.0650(4) -0.2788(2) 0.9213(2) 0.0510(11) Uani 1 1 d . . .
H68A H -0.1065 -0.2814 0.9670 0.077 Uiso 1 1 calc R . .
H68B H -0.1113 -0.2636 0.8810 0.077 Uiso 1 1 calc R . .
H68C H 0.0015 -0.2413 0.9269 0.077 Uiso 1 1 calc R . .
C69 C -0.4518(3) -0.4866(2) 0.8416(2) 0.0327(8) Uani 1 1 d . . .
C70 C -0.4652(3) -0.4225(2) 0.8847(2) 0.0357(9) Uani 1 1 d . . .
C71 C -0.5718(3) -0.4040(2) 0.8934(2) 0.0439(10) Uani 1 1 d . . .
H71 H -0.5818 -0.3609 0.9222 0.053 Uiso 1 1 calc R . .
C72 C -0.6628(3) -0.4468(2) 0.8612(2) 0.0459(11) Uani 1 1 d . . .
H72 H -0.7344 -0.4327 0.8668 0.055 Uiso 1 1 calc R . .
C73 C -0.6493(3) -0.5100(2) 0.8212(2) 0.0432(10) Uani 1 1 d . . .
H73 H -0.7127 -0.5398 0.8002 0.052 Uiso 1 1 calc R . .
C74 C -0.5447(3) -0.5322(2) 0.8099(2) 0.0373(9) Uani 1 1 d . . .
C75 C -0.3660(3) -0.3770(2) 0.9238(2) 0.0417(10) Uani 1 1 d . . .
H75 H -0.3047 -0.3686 0.8877 0.050 Uiso 1 1 calc R . .
C76 C -0.3867(4) -0.2989(2) 0.9516(3) 0.0575(12) Uani 1 1 d . . .
H76A H -0.3194 -0.2732 0.9757 0.086 Uiso 1 1 calc R . .
H76B H -0.4470 -0.3052 0.9868 0.086 Uiso 1 1 calc R . .
H76C H -0.4071 -0.2684 0.9100 0.086 Uiso 1 1 calc R . .
C77 C -0.3255(4) -0.4218(2) 0.9883(2) 0.0486(11) Uani 1 1 d . . .
H77A H -0.2617 -0.3917 1.0124 0.073 Uiso 1 1 calc R . .
H77B H -0.3039 -0.4694 0.9700 0.073 Uiso 1 1 calc R . .
H77C H -0.3850 -0.4331 1.0236 0.073 Uiso 1 1 calc R . .
C78 C -0.5363(3) -0.6025(2) 0.7649(2) 0.0424(10) Uani 1 1 d . . .
H78 H -0.4573 -0.6115 0.7663 0.051 Uiso 1 1 calc R . .
C79 C -0.5695(4) -0.5930(3) 0.6843(2) 0.0605(13) Uani 1 1 d . . .
H79A H -0.5626 -0.6396 0.6571 0.091 Uiso 1 1 calc R . .
H79B H -0.5209 -0.5505 0.6630 0.091 Uiso 1 1 calc R . .
H79C H -0.6463 -0.5827 0.6813 0.091 Uiso 1 1 calc R . .
C80 C -0.6055(4) -0.6726(3) 0.7969(3) 0.0641(14) Uani 1 1 d . . .
H80A H -0.5978 -0.7170 0.7664 0.096 Uiso 1 1 calc R . .
H80B H -0.6833 -0.6648 0.7976 0.096 Uiso 1 1 calc R . .
H80C H -0.5795 -0.6809 0.8471 0.096 Uiso 1 1 calc R . .
C81 C -0.2710(3) -0.5754(2) 0.6466(2) 0.0407(10) Uani 1 1 d . . .
H81A H -0.3332 -0.6096 0.6676 0.049 Uiso 1 1 calc R . .
H81B H -0.2054 -0.5745 0.6795 0.049 Uiso 1 1 calc R . .
C82 C -0.3314(4) -0.4899(2) 0.5600(2) 0.0475(11) Uani 1 1 d . . .
H82A H -0.2776 -0.4513 0.5360 0.057 Uiso 1 1 calc R . .
H82B H -0.4057 -0.4739 0.5560 0.057 Uiso 1 1 calc R . .
C83 C -0.2464(4) -0.6004(2) 0.5709(2) 0.0503(11) Uani 1 1 d . . .
H83A H -0.2567 -0.6564 0.5666 0.060 Uiso 1 1 calc R . .
H83B H -0.1702 -0.5800 0.5567 0.060 Uiso 1 1 calc R . .
C84 C -0.3311(4) -0.5664(2) 0.5251(2) 0.0511(11) Uani 1 1 d . . .
H84A H -0.3091 -0.5617 0.4731 0.061 Uiso 1 1 calc R . .
H84B H -0.4047 -0.5974 0.5279 0.061 Uiso 1 1 calc R . .
N1 N -0.3024(2) -0.97893(17) 0.82749(16) 0.0302(7) Uani 1 1 d . . .
N2 N -0.0720(2) -0.98205(16) 0.77815(16) 0.0296(7) Uani 1 1 d . . .
N3 N -0.1087(2) -0.80248(17) 0.64285(17) 0.0358(7) Uani 1 1 d . . .
N4 N -0.3410(2) -0.49887(16) 0.82503(16) 0.0310(7) Uani 1 1 d . . .
N5 N -0.4165(3) -0.32419(18) 0.70309(17) 0.0385(8) Uani 1 1 d . . .
N6 N -0.1017(2) -0.45647(16) 0.78269(15) 0.0286(7) Uani 1 1 d . . .
O1 O -0.2630(2) -0.99883(13) 0.62977(13) 0.0357(6) Uani 1 1 d . . .
O2 O -0.2999(2) -0.49943(15) 0.63688(14) 0.0417(7) Uiso 1 1 d . . .
Ca1 Ca -0.21078(6) -0.91304(4) 0.72694(4) 0.02923(18) Uani 1 1 d . . .
Ca2 Ca -0.26321(6) -0.41187(4) 0.73390(4) 0.02917(18) Uani 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.2262 0.3064 '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
_geom_angle_publ_flag
C2 C1 Ca1 89.1(2) . . ?
C1 C2 C3 122.9(4) . . ?
C1 C2 C7 122.3(4) . . ?
C3 C2 C7 114.6(4) . . ?
C1 C2 Ca1 61.4(2) . . ?
C3 C2 Ca1 79.6(2) . . ?
C7 C2 Ca1 129.8(3) . . ?
C4 C3 C2 121.4(4) . . ?
C4 C3 N3 121.7(4) . . ?
C2 C3 N3 116.9(3) . . ?
C4 C3 Ca1 134.9(3) . . ?
C2 C3 Ca1 72.4(2) . . ?
N3 C3 Ca1 63.91(18) . . ?
C5 C4 C3 121.6(5) . . ?
C4 C5 C6 118.4(5) . . ?
C7 C6 C5 121.4(4) . . ?
C6 C7 C2 122.6(5) . . ?
N1 C10 C11 124.5(3) . . ?
N1 C10 C14 120.0(3) . . ?
C11 C10 C14 115.4(3) . . ?
C12 C11 C10 129.5(3) . . ?
N2 C12 C11 124.1(3) . . ?
N2 C12 C13 120.9(3) . . ?
C11 C12 C13 115.0(3) . . ?
C16 C15 C20 120.3(3) . . ?
C16 C15 N2 121.7(3) . . ?
C20 C15 N2 117.7(3) . . ?
C16 C15 Ca1 117.5(2) . . ?
C20 C15 Ca1 99.1(2) . . ?
N2 C15 Ca1 45.52(15) . . ?
C17 C16 C15 118.3(3) . . ?
C17 C16 C21 118.7(3) . . ?
C15 C16 C21 122.9(3) . . ?
C18 C17 C16 121.7(4) . . ?
C17 C18 C19 119.8(4) . . ?
C18 C19 C20 120.9(4) . . ?
C19 C20 C15 118.9(3) . . ?
C19 C20 C24 120.6(3) . . ?
C15 C20 C24 120.4(3) . . ?
C16 C21 C23 111.0(3) . . ?
C16 C21 C22 112.5(3) . . ?
C23 C21 C22 109.3(3) . . ?
C25 C24 C26 109.9(4) . . ?
C25 C24 C20 111.0(3) . . ?
C26 C24 C20 113.9(3) . . ?
C32 C27 C28 119.8(3) . . ?
C32 C27 N1 120.9(3) . . ?
C28 C27 N1 119.2(3) . . ?
C32 C27 Ca1 107.1(2) . . ?
C28 C27 Ca1 113.7(2) . . ?
N1 C27 Ca1 42.84(15) . . ?
C29 C28 C27 118.8(3) . . ?
C29 C28 C36 119.6(4) . . ?
C27 C28 C36 121.6(3) . . ?
C30 C29 C28 121.5(4) . . ?
C31 C30 C29 119.1(4) . . ?
C30 C31 C32 121.6(4) . . ?
C31 C32 C27 119.2(4) . . ?
C31 C32 C33 119.6(3) . . ?
C27 C32 C33 121.2(3) . . ?
C34 C33 C35 110.4(4) . . ?
C34 C33 C32 111.4(4) . . ?
C35 C33 C32 111.3(3) . . ?
C38 C36 C28 112.0(3) . . ?
C38 C36 C37 109.1(4) . . ?
C28 C36 C37 111.2(3) . . ?
O1 C39 C42 105.7(3) . . ?
O1 C40 C41 105.3(3) . . ?
C40 C41 C42 104.5(3) . . ?
C39 C42 C41 102.4(3) . . ?
C44 C43 Ca2 85.4(2) . . ?
C43 C44 C45 123.9(4) . . ?
C43 C44 C49 121.7(4) . . ?
C45 C44 C49 114.0(4) . . ?
C43 C44 Ca2 64.3(2) . . ?
C45 C44 Ca2 78.2(2) . . ?
C49 C44 Ca2 127.2(3) . . ?
C46 C45 C44 121.6(3) . . ?
C46 C45 N5 121.8(3) . . ?
C44 C45 N5 116.6(3) . . ?
C46 C45 Ca2 131.7(3) . . ?
C44 C45 Ca2 72.72(19) . . ?
N5 C45 Ca2 66.21(17) . . ?
C47 C46 C45 121.5(4) . . ?
C48 C47 C46 118.6(4) . . ?
C47 C48 C49 121.2(4) . . ?
C48 C49 C44 123.1(4) . . ?
N6 C52 C53 124.9(3) . . ?
N6 C52 C56 119.5(3) . . ?
C53 C52 C56 115.5(3) . . ?
C52 C53 C54 130.3(3) . . ?
N4 C54 C53 124.6(3) . . ?
N4 C54 C55 121.3(3) . . ?
C53 C54 C55 114.0(3) . . ?
C58 C57 C62 120.1(3) . . ?
C58 C57 N6 121.5(3) . . ?
C62 C57 N6 118.3(3) . . ?
C59 C58 C57 118.4(4) . . ?
C59 C58 C63 120.2(4) . . ?
C57 C58 C63 121.4(3) . . ?
C60 C59 C58 121.8(4) . . ?
C61 C60 C59 119.3(4) . . ?
C60 C61 C62 122.1(4) . . ?
C61 C62 C57 118.3(4) . . ?
C61 C62 C66 120.7(4) . . ?
C57 C62 C66 121.0(3) . . ?
C65 C63 C58 110.5(4) . . ?
C65 C63 C64 110.4(4) . . ?
C58 C63 C64 112.7(4) . . ?
C62 C66 C68 110.7(3) . . ?
C62 C66 C67 111.7(4) . . ?
C68 C66 C67 110.4(3) . . ?
C70 C69 C74 120.6(3) . . ?
C70 C69 N4 117.6(3) . . ?
C74 C69 N4 121.4(3) . . ?
C70 C69 Ca2 99.7(2) . . ?
C74 C69 Ca2 117.9(2) . . ?
N4 C69 Ca2 44.17(15) . . ?
C71 C70 C69 118.5(4) . . ?
C71 C70 C75 120.9(4) . . ?
C69 C70 C75 120.6(3) . . ?
C72 C71 C70 121.4(4) . . ?
C73 C72 C71 119.6(4) . . ?
C72 C73 C74 122.3(4) . . ?
C73 C74 C69 117.5(4) . . ?
C73 C74 C78 119.2(3) . . ?
C69 C74 C78 123.2(3) . . ?
C70 C75 C76 114.3(3) . . ?
C70 C75 C77 110.9(3) . . ?
C76 C75 C77 109.0(3) . . ?
C74 C78 C79 112.1(4) . . ?
C74 C78 C80 111.7(3) . . ?
C79 C78 C80 109.9(4) . . ?
02 C81 C83 104.5(3) . . ?
02 C82 C84 105.1(3) . . ?
C81 C83 C84 101.8(3) . . ?
C82 C84 C83 102.9(3) . . ?
C10 N1 C27 117.8(3) . . ?
C10 N1 Ca1 129.2(2) . . ?
C27 N1 Ca1 112.9(2) . . ?
C12 N2 C15 121.0(3) . . ?
C12 N2 Ca1 129.6(2) . . ?
C15 N2 Ca1 109.3(2) . . ?
C3 N3 C8 114.2(3) . . ?
C3 N3 C9 110.9(3) . . ?
C8 N3 C9 107.8(3) . . ?
C3 N3 Ca1 87.0(2) . . ?
C8 N3 Ca1 107.2(2) . . ?
C9 N3 Ca1 128.6(3) . . ?
C54 N4 C69 121.2(3) . . ?
C54 N4 Ca2 127.4(2) . . ?
C69 N4 Ca2 111.0(2) . . ?
C45 N5 C50 114.2(3) . . ?
C45 N5 C51 111.8(3) . . ?
C50 N5 C51 107.9(3) . . ?
C45 N5 Ca2 83.61(19) . . ?
C50 N5 Ca2 108.6(2) . . ?
C51 N5 Ca2 128.9(3) . . ?
C52 N6 C57 118.1(3) . . ?
C52 N6 Ca2 126.5(2) . . ?
C57 N6 Ca2 115.5(2) . . ?
C39 O1 C40 109.1(3) . . ?
C39 O1 Ca1 118.9(2) . . ?
C40 O1 Ca1 131.1(2) . . ?
C81 02 C82 108.9(3) . . ?
C81 02 Ca2 118.6(2) . . ?
C82 02 Ca2 131.6(2) . . ?
O1 Ca1 N1 101.11(10) . . ?
O1 Ca1 N2 95.50(9) . . ?
N1 Ca1 N2 76.84(10) . . ?
O1 Ca1 C1 121.20(13) . . ?
N1 Ca1 C1 99.33(12) . . ?
N2 Ca1 C1 142.88(14) . . ?
O1 Ca1 N3 95.77(9) . . ?
N1 Ca1 N3 162.05(10) . . ?
N2 Ca1 N3 107.75(9) . . ?
C1 Ca1 N3 66.25(12) . . ?
O1 Ca1 C2 94.54(11) . . ?
N1 Ca1 C2 119.83(11) . . ?
N2 Ca1 C2 158.31(11) . . ?
C1 Ca1 C2 29.49(13) . . ?
N3 Ca1 C2 52.02(10) . . ?
O1 Ca1 C3 83.53(10) . . ?
N1 Ca1 C3 147.47(10) . . ?
N2 Ca1 C3 135.21(10) . . ?
C1 Ca1 C3 53.12(12) . . ?
N3 Ca1 C3 29.09(9) . . ?
C2 Ca1 C3 28.00(11) . . ?
O1 Ca1 C15 97.62(9) . . ?
N1 Ca1 C15 101.04(9) . . ?
N2 Ca1 C15 25.17(9) . . ?
C1 Ca1 C15 131.11(13) . . ?
N3 Ca1 C15 82.59(9) . . ?
C2 Ca1 C15 133.96(10) . . ?
C3 Ca1 C15 110.31(10) . . ?
O1 Ca1 C27 107.30(9) . . ?
N1 Ca1 C27 24.27(9) . . ?
N2 Ca1 C27 99.61(9) . . ?
C1 Ca1 C27 76.11(12) . . ?
N3 Ca1 C27 142.15(9) . . ?
C2 Ca1 C27 95.67(10) . . ?
C3 Ca1 C27 123.54(10) . . ?
C15 Ca1 C27 122.12(9) . . ?
02 Ca2 N6 97.93(10) . . ?
02 Ca2 N4 94.15(10) . . ?
N6 Ca2 N4 78.79(10) . . ?
02 Ca2 C43 125.57(13) . . ?
N6 Ca2 C43 97.84(12) . . ?
N4 Ca2 C43 140.02(13) . . ?
02 Ca2 N5 98.94(10) . . ?
N6 Ca2 N5 162.11(10) . . ?
N4 Ca2 N5 105.81(10) . . ?
C43 Ca2 N5 67.30(12) . . ?
02 Ca2 C44 98.33(10) . . ?
N6 Ca2 C44 118.05(10) . . ?
N4 Ca2 C44 157.10(11) . . ?
C43 Ca2 C44 30.26(12) . . ?
N5 Ca2 C44 53.35(10) . . ?
02 Ca2 C45 86.30(10) . . ?
N6 Ca2 C45 146.45(10) . . ?
N4 Ca2 C45 134.33(10) . . ?
C43 Ca2 C45 54.85(11) . . ?
N5 Ca2 C45 30.18(9) . . ?
C44 Ca2 C45 29.06(10) . . ?
02 Ca2 C69 97.53(10) . . ?
N6 Ca2 C69 102.61(10) . . ?
N4 Ca2 C69 24.78(9) . . ?
C43 Ca2 C69 128.71(13) . . ?
N5 Ca2 C69 81.03(9) . . ?
C44 Ca2 C69 133.42(10) . . ?
C45 Ca2 C69 109.83(10) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.421(6) . ?
C1 Ca1 2.535(4) . ?
C2 C3 1.422(5) . ?
C2 C7 1.432(6) . ?
C2 Ca1 2.886(4) . ?
C3 C4 1.398(5) . ?
C3 N3 1.450(5) . ?
C3 Ca1 2.979(4) . ?
C4 C5 1.373(6) . ?
C5 C6 1.382(7) . ?
C6 C7 1.370(7) . ?
C8 N3 1.468(5) . ?
C9 N3 1.470(5) . ?
C10 N1 1.324(5) . ?
C10 C11 1.403(5) . ?
C10 C14 1.520(5) . ?
C11 C12 1.402(5) . ?
C12 N2 1.324(4) . ?
C12 C13 1.521(5) . ?
C15 C16 1.405(5) . ?
C15 C20 1.416(5) . ?
C15 N2 1.432(4) . ?
C15 Ca1 3.177(3) . ?
C16 C17 1.395(5) . ?
C16 C21 1.526(5) . ?
C17 C18 1.377(5) . ?
C18 C19 1.380(6) . ?
C19 C20 1.391(5) . ?
C20 C24 1.534(5) . ?
C21 C23 1.527(5) . ?
C21 C22 1.533(5) . ?
C24 C25 1.518(6) . ?
C24 C26 1.519(6) . ?
C27 C32 1.403(5) . ?
C27 C28 1.409(5) . ?
C27 N1 1.443(4) . ?
C27 Ca1 3.234(3) . ?
C28 C29 1.387(5) . ?
C28 C36 1.522(5) . ?
C29 C30 1.384(5) . ?
C30 C31 1.375(6) . ?
C31 C32 1.386(5) . ?
C32 C33 1.528(6) . ?
C33 C34 1.517(6) . ?
C33 C35 1.528(6) . ?
C36 C38 1.510(6) . ?
C36 C37 1.539(6) . ?
C39 O1 1.448(4) . ?
C39 C42 1.473(5) . ?
C40 O1 1.455(4) . ?
C40 C41 1.515(6) . ?
C41 C42 1.518(6) . ?
C43 C44 1.419(5) . ?
C43 Ca2 2.538(4) . ?
C44 C45 1.428(5) . ?
C44 C49 1.432(6) . ?
C44 Ca2 2.807(4) . ?
C45 C46 1.387(5) . ?
C45 N5 1.456(5) . ?
C45 Ca2 2.878(3) . ?
C46 C47 1.385(5) . ?
C47 C48 1.368(6) . ?
C48 C49 1.369(6) . ?
C50 N5 1.471(5) . ?
C51 N5 1.474(5) . ?
C52 N6 1.338(4) . ?
C52 C53 1.389(5) . ?
C52 C56 1.526(5) . ?
C53 C54 1.416(5) . ?
C54 N4 1.316(4) . ?
C54 C55 1.529(5) . ?
C57 C58 1.410(5) . ?
C57 C62 1.416(5) . ?
C57 N6 1.435(4) . ?
C58 C59 1.392(6) . ?
C58 C63 1.521(6) . ?
C59 C60 1.377(6) . ?
C60 C61 1.370(6) . ?
C61 C62 1.389(5) . ?
C62 C66 1.516(5) . ?
C63 C65 1.517(6) . ?
C63 C64 1.531(6) . ?
C66 C68 1.530(6) . ?
C66 C67 1.532(6) . ?
C69 C70 1.413(5) . ?
C69 C74 1.414(5) . ?
C69 N4 1.438(4) . ?
C69 Ca2 3.202(3) . ?
C70 C71 1.399(5) . ?
C70 C75 1.526(5) . ?
C71 C72 1.379(6) . ?
C72 C73 1.368(6) . ?
C73 C74 1.407(5) . ?
C74 C78 1.510(5) . ?
C75 C76 1.532(6) . ?
C75 C77 1.533(6) . ?
C78 C79 1.530(6) . ?
C78 C80 1.530(6) . ?
C81 02 1.454(4) . ?
C81 C83 1.495(5) . ?
C82 02 1.462(4) . ?
C82 C84 1.502(6) . ?
C83 C84 1.507(6) . ?
N1 Ca1 2.387(3) . ?
N2 Ca1 2.402(3) . ?
N3 Ca1 2.679(3) . ?
N4 Ca2 2.390(3) . ?
N5 Ca2 2.650(3) . ?
N6 Ca2 2.383(3) . ?
O1 Ca1 2.355(3) . ?
02 Ca2 2.349(3) . ?
