#------------------------------------------------------------------------------
#$Date: 2023-04-04 12:46:11 +0300 (Tue, 04 Apr 2023) $
#$Revision: 282266 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/13/14/7131430.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_7131430
loop_
_publ_author_name
'Muang-Non, Phonlakrit'
'Markwell-Heys, Adrian W'
'Doonan, Christian J.'
'White, Nicholas G.'
_publ_section_title
;
 Charge "mis-matched" hydrogen bonded frameworks for cation exchange and
 dye sorption.
;
_journal_issue                   27
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4059
_journal_page_last               4062
_journal_paper_doi               10.1039/d3cc00553d
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety
'H12 Na O6, C28 H16 B O8, 4(H2 O), 2(C14 H16 N4)'
_chemical_formula_sum            'C56 H68 B N8 Na O18'
_chemical_formula_weight         1174.98
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-01-11
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-01-31 deposited with the CCDC.	2023-03-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.871(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.2633(6)
_cell_length_b                   14.7730(5)
_cell_length_c                   19.7937(7)
_cell_measurement_reflns_used    4137
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      60.8430
_cell_measurement_theta_min      3.7460
_cell_volume                     5625.8(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -85.00  -6.00   1.00   15.00    --  -36.63 125.00-150.00   79
  2  ω   -100.00 -21.00   1.00   15.00    --  -36.63 -57.00  60.00   79
  3  ω    110.00 150.00   1.00   80.00    --   84.58  77.00-150.00   40
  4  ω     19.00  99.00   1.00   80.00    --   84.58 -61.00 -30.00   80
  5  ω    112.00 152.00   1.00   80.00    --   84.58  77.00 -60.00   40
  6  ω     99.00 133.00   1.00   80.00    --   84.58 125.00 150.00   34
  7  ω    102.00 144.00   1.00   80.00    --   84.58 125.00-150.00   42
  8  ω    104.00 154.00   1.00   80.00    --   84.58 125.00  60.00   50
  9  ω    103.00 149.00   1.00   80.00    --   84.58  77.00  60.00   46
 10  ω     76.00 154.00   1.00   80.00    --   84.58  30.00-150.00   78
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0337851000
_diffrn_orient_matrix_UB_12      0.0860578000
_diffrn_orient_matrix_UB_13      0.0309160000
_diffrn_orient_matrix_UB_21      -0.0703809000
_diffrn_orient_matrix_UB_22      0.0282446000
_diffrn_orient_matrix_UB_23      0.0269918000
_diffrn_orient_matrix_UB_31      0.0177683000
_diffrn_orient_matrix_UB_32      -0.0516804000
_diffrn_orient_matrix_UB_33      0.0662635000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_unetI/netI     0.0522
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15878
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        58.932
_diffrn_reflns_theta_max         58.932
_diffrn_reflns_theta_min         3.735
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.933
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73137
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.387
_exptl_crystal_description       needle
_exptl_crystal_F_000             2480
_exptl_crystal_recrystallization_method
'Crystallised using diphenylbisamidinium.2Cl with TBA5.tetraboratecarboxylate in 50% EtOH with 100 equivalent of NaCl. Final concentration = 2 mM.'
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.855
_refine_diff_density_min         -0.689
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     836
_refine_ls_number_reflns         8008
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1028
_refine_ls_R_factor_gt           0.0804
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0947P)²+14.1103P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2017
_refine_ls_wR_factor_ref         0.2196
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6149
_reflns_number_total             8008
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3cc00553d2.cif
_cod_data_source_block           Na_2_B
_cod_depositor_comments
'Adding full bibliography for 7131429--7131437.cif.'
_cod_database_code               7131430
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C50H50B20N25O50
_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.
;
_shelx_estimated_absorpt_t_max   0.955
_shelx_estimated_absorpt_t_min   0.668
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O130-H13C = O130-H13D
 0.87 with sigma of 0.02
 O150-H15A = O150-H15B
 0.87 with sigma of 0.02
 O140-H14A = O140-H14B
 0.87 with sigma of 0.02
 H13C-H13D
 1.38 with sigma of 0.04
 H15A-H15B
 1.38 with sigma of 0.04
 H14A-H14B
 1.38 with sigma of 0.04
 Na1-H16A \\sim Na1-H16B
 with sigma of 0.02
 Na1-H15A \\sim Na1-H15B
 with sigma of 0.02
 Na1-H14A \\sim Na1-H14B
 with sigma of 0.02
3. Others
 Fixed Sof: O100(0.5) H10C(0.5) H10D(0.5) O150(0.6666) H15A(0.6666)
 H15B(0.6666) O110(0.5) H11C(0.5) H11D(0.5) O160(0.33333) H16A(0.33333)
 H16B(0.33333) O130(0.75) H13C(0.75) H13D(0.75) O9(0.25) H9A(0.25) H9B(0.25)
 O10(0.5) H10E(0.5) H10F(0.5) O11(0.5) H11E(0.5) H11F(0.5)
4.a Free rotating group:
 O120(H12C,H12D), O200(H20A,H20B), O110(H11C,H11D), O160(H16A,H16B), O9(H9A,
 H9B), O10(H10E,H10F), O11(H11E,H11F)
4.b Rotating group:
 O180(H18A,H18B), O190(H19A,H19B), O170(H17A,H17B), O100(H10C,H10D)
4.c Aromatic/amide H refined with riding coordinates:
 C53(H53), C52(H52), C43(H43), C50(H50), C59(H59), C56(H56), C57(H57), C7(H7),
 C6(H6), C64(H64), C9(H9), C49(H49), C42(H42), C67(H67), C12(H12), C10(H10),
 C45(H45), C14(H14), C63(H63), C66(H66), C60(H60), C3(H3), C4(H4), C46(H46),
 C31(H31), C22(H22), C32(H32), C23(H23), C26(H26), C25(H25), C28(H28), C29(H29)
4.d X=CH2 refined with riding coordinates:
 N4(H4A,H4B), N3(H3A,H3B), N11(H11A,H11B), N1(H1A,H1B), N10(H10A,H10B), N2(H2A,
 H2B), N13(H13A,H13B), N12(H12A,H12B)
;
_ins_header
;
TITL PMN-C-21-NaCl-repro in P2(1)/n 
REM P2(1)/n (#14 in standard setting)
CELL 1.54184  19.263310  14.773009  19.793722  90.0000  92.8710  90.0000
ZERR    2.00   0.000620   0.000452   0.000744   0.0000   0.0034   0.0000
LATT  1
SYMM -x+1/2, y+1/2,-z+1/2 
SFAC C H B N O
UNIT 100.00 100.00 40.00 50.00 100.00
REM  CrysAlisPro recorded range (K): Min=150.0; max=150.0; aver:150.0
TEMP -123
SIZE 0.05 0.10 0.47
TREF
HKLF 4
END
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.469
_oxdiff_exptl_absorpt_empirical_full_min 0.681
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
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Na1 Na 0.76867(13) 0.31603(16) 0.25677(13) 0.0651(7) Uani 1 1 d D . . . .
O5 O 0.51030(16) 0.76839(19) 0.26080(17) 0.0380(8) Uani 1 1 d . . . . .
O4 O -0.00890(17) 0.8264(2) 0.24342(18) 0.0411(8) Uani 1 1 d . . . . .
O6 O 0.56196(16) 0.6398(2) 0.23438(18) 0.0416(8) Uani 1 1 d . . . . .
O120 O 0.59589(18) 0.4671(2) 0.20575(18) 0.0442(9) Uani 1 1 d G . . . .
H12C H 0.584246 0.518418 0.223556 0.066 Uiso 1 1 d G U . . .
H12D H 0.570622 0.427048 0.225332 0.066 Uiso 1 1 d G U . . .
O3 O -0.07368(17) 0.7070(2) 0.26613(19) 0.0472(9) Uani 1 1 d . . . . .
O200 O 0.78807(19) 0.4333(2) 0.10050(19) 0.0487(9) Uani 1 1 d G . . . .
H20A H 0.763772 0.393655 0.076993 0.073 Uiso 1 1 d G U . . .
H20B H 0.771782 0.485331 0.086692 0.073 Uiso 1 1 d G U . . .
O2 O 0.25659(18) 0.3076(2) 0.56371(18) 0.0463(9) Uani 1 1 d . . . . .
O7 O 0.2401(2) 0.3891(2) -0.07004(19) 0.0542(10) Uani 1 1 d . . . . .
O1 O 0.2149(2) 0.1880(2) 0.5073(2) 0.0549(10) Uani 1 1 d . . . . .
O180 O 0.8401(2) 0.2457(2) 0.1787(2) 0.0536(10) Uani 1 1 d . . . . .
H18A H 0.814309 0.220350 0.146308 0.080 Uiso 1 1 d R U . . .
H18B H 0.862393 0.200400 0.198321 0.080 Uiso 1 1 d R U . . .
N4 N 0.5722(2) 0.8917(3) 0.3666(2) 0.0369(9) Uani 1 1 d . . . . .
H4A H 0.573329 0.838987 0.345888 0.044 Uiso 1 1 calc R U . . .
H4B H 0.610597 0.914612 0.385543 0.044 Uiso 1 1 calc R U . . .
O190 O 0.8167(2) 0.2046(3) 0.3327(2) 0.0600(11) Uani 1 1 d . . . . .
H19A H 0.789848 0.155228 0.332378 0.090 Uiso 1 1 d R U . . .
H19B H 0.857014 0.183967 0.318408 0.090 Uiso 1 1 d R U . . .
N3 N 0.4563(2) 0.9007(3) 0.3404(2) 0.0386(9) Uani 1 1 d . . . . .
H3A H 0.457832 0.848015 0.319855 0.046 Uiso 1 1 calc R U . . .
H3B H 0.416600 0.930004 0.341908 0.046 Uiso 1 1 calc R U . . .
O8 O 0.2414(3) 0.2508(2) -0.0285(2) 0.0694(14) Uani 1 1 d . . . . .
O170 O 0.6780(2) 0.2883(3) 0.1628(2) 0.0669(13) Uani 1 1 d . . . . .
H17A H 0.641995 0.261411 0.179077 0.100 Uiso 1 1 d R U . . .
H17B H 0.693814 0.249193 0.134216 0.100 Uiso 1 1 d R U . . .
N11 N 0.1361(2) 0.0499(3) 0.4556(2) 0.0439(10) Uani 1 1 d . . . . .
H11A H 0.155826 0.103586 0.457276 0.053 Uiso 1 1 calc R U . . .
H11B H 0.132537 0.020017 0.417063 0.053 Uiso 1 1 calc R U . . .
N1 N 0.4261(2) 1.5607(3) 0.6279(2) 0.0495(11) Uani 1 1 d . . . . .
H1A H 0.422625 1.610834 0.651555 0.059 Uiso 1 1 calc R U . . .
H1B H 0.388495 1.534791 0.609789 0.059 Uiso 1 1 calc R U . . .
N10 N 0.1176(2) 0.0595(3) 0.5671(2) 0.0486(11) Uani 1 1 d . . . . .
H10A H 0.137440 0.113164 0.568065 0.058 Uiso 1 1 calc R U . . .
H10B H 0.101582 0.036521 0.604301 0.058 Uiso 1 1 calc R U . . .
N2 N 0.5434(2) 1.5622(3) 0.6462(2) 0.0474(11) Uani 1 1 d . . . . .
H2A H 0.540667 1.612288 0.669985 0.057 Uiso 1 1 calc R U . . .
H2B H 0.584100 1.537224 0.640340 0.057 Uiso 1 1 calc R U . . .
O140 O 0.6699(2) 0.2945(3) 0.3338(2) 0.0745(13) Uani 1 1 d D . . . .
H14A H 0.644(3) 0.244(3) 0.327(3) 0.112 Uiso 1 1 d D U . . .
H14B H 0.684(3) 0.280(5) 0.3769(16) 0.112 Uiso 1 1 d D U . . .
C44 C 0.2243(2) 0.4446(3) 0.1832(2) 0.0274(10) Uani 1 1 d . . . . .
C53 C 0.3876(2) 0.6711(3) 0.2893(2) 0.0288(10) Uani 1 1 d . . . . .
H53 H 0.395147 0.725498 0.314289 0.035 Uiso 1 1 calc R U . . .
C52 C 0.3248(2) 0.6272(3) 0.2913(2) 0.0297(10) Uani 1 1 d . . . . .
H52 H 0.290401 0.652305 0.318495 0.036 Uiso 1 1 calc R U . . .
C65 C 0.2339(2) 0.4285(3) 0.3228(2) 0.0260(9) Uani 1 1 d . . . . .
C48 C 0.4404(2) 0.6366(3) 0.2511(2) 0.0283(10) Uani 1 1 d . . . . .
C5 C 0.5002(2) 1.2768(3) 0.5091(2) 0.0292(10) Uani 1 1 d . . . . .
C58 C 0.1674(2) 0.5677(3) 0.2618(2) 0.0279(10) Uani 1 1 d . . . . .
C43 C 0.2127(2) 0.4968(3) 0.1244(2) 0.0296(10) Uani 1 1 d . . . . .
H43 H 0.201303 0.558931 0.129494 0.035 Uiso 1 1 calc R U . . .
N13 N -0.1474(3) -0.6276(3) 0.4232(3) 0.0585(14) Uani 1 1 d . . . . .
H13A H -0.170956 -0.678661 0.420883 0.070 Uiso 1 1 calc R U . . .
H13B H -0.124008 -0.609763 0.388485 0.070 Uiso 1 1 calc R U . . .
C50 C 0.3636(2) 0.5137(3) 0.2186(2) 0.0325(10) Uani 1 1 d . . . . .
H50 H 0.356431 0.459095 0.193940 0.039 Uiso 1 1 calc R U . . .
C59 C 0.1034(2) 0.5397(3) 0.2841(2) 0.0299(10) Uani 1 1 d . . . . .
H59 H 0.099429 0.479652 0.300738 0.036 Uiso 1 1 calc R U . . .
C56 C 0.1125(2) 0.7158(3) 0.2412(2) 0.0305(10) Uani 1 1 d . . . . .
H56 H 0.117007 0.777041 0.227536 0.037 Uiso 1 1 calc R U . . .
C2 C 0.4918(2) 1.4397(3) 0.5805(2) 0.0292(10) Uani 1 1 d . . . . .
C11 C 0.5109(2) 1.0244(3) 0.4039(2) 0.0317(10) Uani 1 1 d . . . . .
C57 C 0.1695(2) 0.6588(3) 0.2403(2) 0.0285(10) Uani 1 1 d . . . . .
H57 H 0.211822 0.681935 0.224642 0.034 Uiso 1 1 calc R U . . .
C8 C 0.5046(2) 1.1897(3) 0.4716(2) 0.0296(10) Uani 1 1 d . . . . .
C62 C 0.2349(2) 0.3221(3) 0.4444(2) 0.0324(11) Uani 1 1 d . . . . .
C7 C 0.5547(2) 1.4126(3) 0.5547(2) 0.0325(10) Uani 1 1 d . . . . .
H7 H 0.594656 1.449999 0.560717 0.039 Uiso 1 1 calc R U . . .
C51 C 0.3086(2) 0.5477(3) 0.2554(2) 0.0279(10) Uani 1 1 d . . . . .
C6 C 0.5588(2) 1.3314(3) 0.5204(2) 0.0337(11) Uani 1 1 d . . . . .
H6 H 0.602047 1.312460 0.504235 0.040 Uiso 1 1 calc R U . . .
C64 C 0.1961(2) 0.3474(3) 0.3277(2) 0.0323(10) Uani 1 1 d . . . . .
H64 H 0.168727 0.327501 0.289241 0.039 Uiso 1 1 calc R U . . .
C55 C 0.0485(2) 0.6846(3) 0.2618(2) 0.0323(10) Uani 1 1 d . . . . .
C15 C 0.5135(2) 0.9359(3) 0.3691(2) 0.0324(10) Uani 1 1 d . . . . .
C47 C 0.5091(2) 0.6847(3) 0.2486(2) 0.0314(10) Uani 1 1 d . . . . .
C9 C 0.4519(2) 1.1645(3) 0.4247(2) 0.0350(11) Uani 1 1 d . . . . .
H9 H 0.413244 1.203533 0.415987 0.042 Uiso 1 1 calc R U . . .
C54 C -0.0153(2) 0.7437(3) 0.2569(2) 0.0357(11) Uani 1 1 d . . . . .
C1 C 0.4870(2) 1.5249(3) 0.6198(2) 0.0335(11) Uani 1 1 d . . . . .
O100 O -0.1077(5) -0.6080(9) 0.2863(7) 0.039(2) Uani 0.5 1 d . . P A 1
H10C H -0.099483 -0.549792 0.261721 0.058 Uiso 0.5 1 d R U P A 1
H10D H -0.067682 -0.643749 0.270994 0.058 Uiso 0.5 1 d R U P A 1
C49 C 0.4272(2) 0.5557(3) 0.2167(2) 0.0349(11) Uani 1 1 d . . . . .
H49 H 0.462636 0.529063 0.191559 0.042 Uiso 1 1 calc R U . . .
C41 C 0.2321(2) 0.3722(3) 0.0491(2) 0.0336(11) Uani 1 1 d . . . . .
C42 C 0.2168(2) 0.4635(3) 0.0599(2) 0.0313(10) Uani 1 1 d . . . . .
H42 H 0.209114 0.502813 0.022219 0.038 Uiso 1 1 calc R U . . .
C67 C 0.2723(2) 0.4025(3) 0.4420(2) 0.0344(11) Uani 1 1 d . . . . .
H67 H 0.298186 0.423271 0.481027 0.041 Uiso 1 1 calc R U . . .
C12 C 0.5635(2) 1.0489(3) 0.4509(2) 0.0348(11) Uani 1 1 d . . . . .
H12 H 0.601516 1.009167 0.460533 0.042 Uiso 1 1 calc R U . . .
C10 C 0.4554(2) 1.0827(3) 0.3905(2) 0.0343(11) Uani 1 1 d . . . . .
H10 H 0.419689 1.066578 0.357911 0.041 Uiso 1 1 calc R U . . .
C45 C 0.2384(2) 0.3533(3) 0.1708(3) 0.0369(11) Uani 1 1 d . . . . .
H45 H 0.246007 0.313734 0.208238 0.044 Uiso 1 1 calc R U . . .
C30 C 0.0768(2) -0.0758(3) 0.5068(3) 0.0396(12) Uani 1 1 d . . . . .
C14 C 0.5605(2) 1.1319(3) 0.4839(2) 0.0347(11) Uani 1 1 d . . . . .
H14 H 0.597077 1.149109 0.515204 0.042 Uiso 1 1 calc R U . . .
C63 C 0.1970(2) 0.2950(3) 0.3861(2) 0.0339(11) Uani 1 1 d . . . . .
H63 H 0.171463 0.239978 0.386317 0.041 Uiso 1 1 calc R U . . .
C66 C 0.2718(2) 0.4528(3) 0.3823(2) 0.0318(10) Uani 1 1 d . . . . .
H66 H 0.298712 0.506639 0.381978 0.038 Uiso 1 1 calc R U . . .
C60 C 0.0452(2) 0.5947(3) 0.2833(2) 0.0353(11) Uani 1 1 d . . . . .
H60 H 0.002431 0.571072 0.297486 0.042 Uiso 1 1 calc R U . . .
C33 C 0.1118(2) 0.0141(3) 0.5106(3) 0.0396(12) Uani 1 1 d . . . . .
C3 C 0.4338(2) 1.3856(3) 0.5693(3) 0.0381(11) Uani 1 1 d . . . . .
H3 H 0.390664 1.403567 0.586343 0.046 Uiso 1 1 calc R U . . .
C4 C 0.4380(2) 1.3054(3) 0.5336(3) 0.0375(11) Uani 1 1 d . . . . .
H4 H 0.397442 1.269554 0.525721 0.045 Uiso 1 1 calc R U . . .
C61 C 0.2355(3) 0.2689(3) 0.5097(3) 0.0403(12) Uani 1 1 d . . . . .
C46 C 0.2418(3) 0.3181(3) 0.1059(3) 0.0409(12) Uani 1 1 d . . . . .
H46 H 0.250879 0.255415 0.100441 0.049 Uiso 1 1 calc R U . . .
C27 C 0.0065(3) -0.2434(3) 0.4996(3) 0.0421(13) Uani 1 1 d . . . . .
O150 O 0.7384(3) 0.4707(3) 0.2620(3) 0.0440(13) Uani 0.6666 1 d D . P B 1
H15A H 0.6957(14) 0.494(3) 0.259(5) 0.066 Uiso 0.6666 1 d D U P C 1
H15B H 0.760(2) 0.520(2) 0.250(4) 0.066 Uiso 0.6666 1 d D U P D 1
C31 C 0.0408(3) -0.1080(4) 0.5616(3) 0.0429(12) Uani 1 1 d . . . . .
H31 H 0.039820 -0.073122 0.601896 0.051 Uiso 1 1 calc R U . . .
N12 N -0.1822(3) -0.6065(3) 0.5291(3) 0.081(2) Uani 1 1 d . . . . .
H12A H -0.205681 -0.657532 0.526482 0.097 Uiso 1 1 calc R U . . .
H12B H -0.182179 -0.573645 0.566203 0.097 Uiso 1 1 calc R U . . .
C40 C 0.2386(3) 0.3349(3) -0.0214(3) 0.0443(13) Uani 1 1 d . . . . .
C24 C -0.0322(3) -0.3302(3) 0.4942(3) 0.0451(14) Uani 1 1 d . . . . .
C21 C -0.1079(3) -0.4933(3) 0.4827(3) 0.0492(15) Uani 1 1 d . . . . .
C22 C -0.0992(3) -0.4395(3) 0.4259(3) 0.0491(14) Uani 1 1 d . . . . .
H22 H -0.118825 -0.457590 0.383040 0.059 Uiso 1 1 calc R U . . .
C32 C 0.0066(3) -0.1903(4) 0.5573(3) 0.0445(13) Uani 1 1 d . . . . .
H32 H -0.017471 -0.211040 0.595068 0.053 Uiso 1 1 calc R U . . .
C23 C -0.0618(3) -0.3592(3) 0.4323(3) 0.0470(14) Uani 1 1 d . . . . .
H23 H -0.056228 -0.323100 0.393218 0.056 Uiso 1 1 calc R U . . .
C26 C -0.0786(3) -0.4661(3) 0.5438(3) 0.0559(17) Uani 1 1 d . . . . .
H26 H -0.083838 -0.503176 0.582434 0.067 Uiso 1 1 calc R U . . .
C25 C -0.0409(3) -0.3850(3) 0.5511(3) 0.0507(15) Uani 1 1 d . . . . .
H25 H -0.021462 -0.367327 0.594133 0.061 Uiso 1 1 calc R U . . .
O110 O -0.1470(5) 0.5576(7) 0.2068(5) 0.041(2) Uani 0.5 1 d G . P E 1
H11C H -0.122135 0.600645 0.225769 0.062 Uiso 0.5 1 d G U P E 1
H11D H -0.145695 0.568171 0.163618 0.062 Uiso 0.5 1 d G U P E 1
C28 C 0.0447(3) -0.2117(4) 0.4462(3) 0.0584(17) Uani 1 1 d . . . . .
H28 H 0.046957 -0.246934 0.406210 0.070 Uiso 1 1 calc R U . . .
C29 C 0.0792(3) -0.1297(3) 0.4509(3) 0.0549(16) Uani 1 1 d . . . . .
H29 H 0.105309 -0.110265 0.414085 0.066 Uiso 1 1 calc R U . . .
B1 B 0.2329(2) 0.4955(3) 0.2566(3) 0.0282(11) Uani 1 1 d . . . . .
C20 C -0.1470(3) -0.5791(3) 0.4774(3) 0.0576(17) Uani 1 1 d . . . . .
O160 O 0.7136(5) 0.4213(9) 0.1981(5) 0.053(3) Uani 0.3333 1 d G . P B 2
H16A H 0.675019 0.421663 0.219060 0.080 Uiso 0.3333 1 d DG U P B 2
H16B H 0.736439 0.468155 0.213908 0.080 Uiso 0.3333 1 d DG U P B 2
O130 O 0.7158(3) 0.5145(4) 0.3951(3) 0.0543(13) Uani 0.75 1 d D . P F 1
H13C H 0.717(5) 0.480(5) 0.360(3) 0.081 Uiso 0.75 1 d D U P G 1
H13D H 0.745(4) 0.556(4) 0.381(4) 0.081 Uiso 0.75 1 d D U P H 1
O9 O 0.6880(9) 0.4208(13) 0.4544(10) 0.072(5) Uani 0.25 1 d G . P I 2
H9A H 0.713323 0.454598 0.429302 0.109 Uiso 0.25 1 d G U P I 2
H9B H 0.645467 0.432205 0.440188 0.109 Uiso 0.25 1 d G U P I 2
O10 O -0.1269(11) 0.5493(11) 0.2416(12) 0.129(7) Uani 0.5 1 d G . P J 2
H10E H -0.162361 0.556658 0.266626 0.194 Uiso 0.5 1 d G U P J 2
H10F H -0.103384 0.599358 0.246541 0.194 Uiso 0.5 1 d G U P J 2
O11 O -0.0779(10) -0.5985(10) 0.3081(8) 0.098(6) Uani 0.5 1 d G . P K 2
H11E H -0.055485 -0.646276 0.295510 0.147 Uiso 0.5 1 d G U P K 2
H11F H -0.114967 -0.597001 0.281122 0.147 Uiso 0.5 1 d G U P K 2
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'
B B 0.0090 0.0039 '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'
Na Na 0.1353 0.1239 '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'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-5 0 12 0.0078
6 0 -12 0.0365
-5 -9 3 0.1890
6 0 11 0.0225
-6 1 -11 0.0338
-6 -1 -11 0.0353
5 9 -3 0.1838
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
O180 Na1 O190 83.59(15) . . ?
O180 Na1 O170 81.43(15) . . ?
O180 Na1 O140 145.51(18) . . ?
O180 Na1 O100 77.6(3) . 1_665 ?
O180 Na1 O150 127.42(19) . . ?
O180 Na1 H16A 121.4 . . ?
O180 Na1 H16B 108.7 . . ?
O190 Na1 O170 125.86(17) . . ?
O190 Na1 O140 79.19(16) . . ?
O190 Na1 O100 80.7(3) . 1_665 ?
O190 Na1 H16A 151.7 . . ?
O190 Na1 H16B 158.0 . . ?
O170 Na1 O100 143.8(3) . 1_665 ?
O170 Na1 H16A 53.9 . . ?
O170 Na1 H16B 75.0 . . ?
O140 Na1 O170 84.80(16) . . ?
O140 Na1 O100 127.8(3) . 1_665 ?
O140 Na1 H16A 72.6 . . ?
O140 Na1 H16B 97.9 . . ?
O150 Na1 O190 136.8(2) . . ?
O150 Na1 O170 91.50(19) . . ?
O150 Na1 O140 84.23(18) . . ?
O150 Na1 O100 78.6(3) . 1_665 ?
O160 Na1 O180 104.4(3) . . ?
O160 Na1 O190 171.8(3) . . ?
O160 Na1 O170 54.8(3) . . ?
O160 Na1 O140 92.9(3) . . ?
O160 Na1 O100 102.8(4) . 1_665 ?
O160 Na1 H16A 20.3 . . ?
O160 Na1 H16B 20.4 . . ?
H16A Na1 H16B 32.3 . . ?
H12C O120 H12D 104.5 . . ?
H20A O200 H20B 104.5 . . ?
Na1 O180 H18A 109.8 . . ?
Na1 O180 H18B 109.5 . . ?
H18A O180 H18B 104.2 . . ?
H4A N4 H4B 120.0 . . ?
C15 N4 H4A 120.0 . . ?
C15 N4 H4B 120.0 . . ?
Na1 O190 H19A 110.6 . . ?
Na1 O190 H19B 110.6 . . ?
H19A O190 H19B 103.4 . . ?
H3A N3 H3B 120.0 . . ?
C15 N3 H3A 120.0 . . ?
C15 N3 H3B 120.0 . . ?
Na1 O170 H17A 109.6 . . ?
Na1 O170 H17B 109.5 . . ?
H17A O170 H17B 104.3 . . ?
H11A N11 H11B 120.0 . . ?
C33 N11 H11A 120.0 . . ?
C33 N11 H11B 120.0 . . ?
H1A N1 H1B 120.0 . . ?
C1 N1 H1A 120.0 . . ?
C1 N1 H1B 120.0 . . ?
H10A N10 H10B 120.0 . . ?
C33 N10 H10A 120.0 . . ?
C33 N10 H10B 120.0 . . ?
H2A N2 H2B 120.0 . . ?
C1 N2 H2A 120.0 . . ?
C1 N2 H2B 120.0 . . ?
Na1 O140 H14A 116(4) . . ?
Na1 O140 H14B 114(4) . . ?
H14A O140 H14B 94(4) . . ?
C43 C44 B1 119.2(3) . . ?
C45 C44 C43 114.0(4) . . ?
C45 C44 B1 125.9(4) . . ?
C52 C53 H53 119.7 . . ?
C52 C53 C48 120.6(4) . . ?
C48 C53 H53 119.7 . . ?
C53 C52 H52 118.1 . . ?
C53 C52 C51 123.8(4) . . ?
C51 C52 H52 118.1 . . ?
C64 C65 B1 125.6(4) . . ?
C66 C65 C64 114.2(4) . . ?
C66 C65 B1 120.1(4) . . ?
C53 C48 C47 120.8(4) . . ?
C49 C48 C53 117.3(4) . . ?
C49 C48 C47 121.9(4) . . ?
C6 C5 C8 120.8(4) . . ?
C4 C5 C8 120.8(4) . . ?
C4 C5 C6 118.4(4) . . ?
C59 C58 C57 114.7(4) . . ?
C59 C58 B1 121.1(4) . . ?
C57 C58 B1 124.0(4) . . ?
C44 C43 H43 118.0 . . ?
C42 C43 C44 124.0(4) . . ?
C42 C43 H43 118.0 . . ?
H13A N13 H13B 120.0 . . ?
C20 N13 H13A 120.0 . . ?
C20 N13 H13B 120.0 . . ?
C51 C50 H50 118.4 . . ?
C49 C50 H50 118.4 . . ?
C49 C50 C51 123.3(4) . . ?
C58 C59 H59 118.3 . . ?
C60 C59 C58 123.4(4) . . ?
C60 C59 H59 118.3 . . ?
C57 C56 H56 119.5 . . ?
C57 C56 C55 121.1(4) . . ?
C55 C56 H56 119.5 . . ?
C7 C2 C1 120.8(4) . . ?
C3 C2 C7 119.0(4) . . ?
C3 C2 C1 120.2(4) . . ?
C12 C11 C15 120.1(4) . . ?
C10 C11 C15 120.2(4) . . ?
C10 C11 C12 119.7(4) . . ?
C58 C57 H57 118.7 . . ?
C56 C57 C58 122.7(4) . . ?
C56 C57 H57 118.7 . . ?
C9 C8 C5 120.4(4) . . ?
C14 C8 C5 120.6(4) . . ?
C14 C8 C9 119.1(4) . . ?
C67 C62 C63 117.9(4) . . ?
C67 C62 C61 119.5(5) . . ?
C63 C62 C61 122.6(4) . . ?
C2 C7 H7 120.0 . . ?
C6 C7 C2 119.9(4) . . ?
C6 C7 H7 120.0 . . ?
C52 C51 C50 114.0(4) . . ?
C52 C51 B1 124.1(4) . . ?
C50 C51 B1 121.9(4) . . ?
C5 C6 H6 119.5 . . ?
C7 C6 C5 121.0(4) . . ?
C7 C6 H6 119.5 . . ?
C65 C64 H64 118.5 . . ?
C63 C64 C65 123.0(4) . . ?
C63 C64 H64 118.5 . . ?
C56 C55 C54 121.3(4) . . ?
C56 C55 C60 117.2(4) . . ?
C60 C55 C54 121.4(4) . . ?
N4 C15 N3 119.4(4) . . ?
N4 C15 C11 120.5(4) . . ?
N3 C15 C11 120.1(4) . . ?
O5 C47 C48 117.7(4) . . ?
O6 C47 O5 123.5(4) . . ?
O6 C47 C48 118.8(4) . . ?
C8 C9 H9 119.8 . . ?
C10 C9 C8 120.4(4) . . ?
C10 C9 H9 119.8 . . ?
O4 C54 O3 122.8(4) . . ?
O4 C54 C55 119.2(4) . . ?
O3 C54 C55 118.0(4) . . ?
N1 C1 C2 119.2(4) . . ?
N2 C1 N1 121.0(4) . . ?
N2 C1 C2 119.8(4) . . ?
Na1 O100 H10C 114.5 1_445 . ?
Na1 O100 H10D 114.0 1_445 . ?
H10C O100 H10D 99.4 . . ?
C48 C49 H49 119.5 . . ?
C50 C49 C48 120.9(4) . . ?
C50 C49 H49 119.5 . . ?
C42 C41 C40 121.2(4) . . ?
C46 C41 C42 117.0(4) . . ?
C46 C41 C40 121.8(4) . . ?
C43 C42 C41 120.5(4) . . ?
C43 C42 H42 119.7 . . ?
C41 C42 H42 119.7 . . ?
C62 C67 H67 119.9 . . ?
C62 C67 C66 120.2(4) . . ?
C66 C67 H67 119.9 . . ?
C11 C12 H12 120.1 . . ?
C11 C12 C14 119.8(4) . . ?
C14 C12 H12 120.1 . . ?
C11 C10 H10 119.9 . . ?
C9 C10 C11 120.2(4) . . ?
C9 C10 H10 119.9 . . ?
C44 C45 H45 118.6 . . ?
C46 C45 C44 122.8(4) . . ?
C46 C45 H45 118.6 . . ?
C31 C30 C33 120.3(5) . . ?
C29 C30 C33 121.8(4) . . ?
C29 C30 C31 118.0(5) . . ?
C8 C14 C12 120.8(4) . . ?
C8 C14 H14 119.6 . . ?
C12 C14 H14 119.6 . . ?
C62 C63 C64 120.8(4) . . ?
C62 C63 H63 119.6 . . ?
C64 C63 H63 119.6 . . ?
C65 C66 H66 118.1 . . ?
C67 C66 C65 123.8(4) . . ?
C67 C66 H66 118.1 . . ?
C59 C60 C55 120.8(4) . . ?
C59 C60 H60 119.6 . . ?
C55 C60 H60 119.6 . . ?
N11 C33 C30 119.6(5) . . ?
N10 C33 N11 119.0(5) . . ?
N10 C33 C30 121.4(4) . . ?
C2 C3 H3 119.7 . . ?
C2 C3 C4 120.6(4) . . ?
C4 C3 H3 119.7 . . ?
C5 C4 C3 121.0(4) . . ?
C5 C4 H4 119.5 . . ?
C3 C4 H4 119.5 . . ?
O2 C61 C62 118.5(4) . . ?
O1 C61 O2 123.3(5) . . ?
O1 C61 C62 118.2(5) . . ?
C41 C46 C45 121.6(4) . . ?
C41 C46 H46 119.2 . . ?
C45 C46 H46 119.2 . . ?
C32 C27 C24 121.8(4) . . ?
C32 C27 C28 117.0(5) . . ?
C28 C27 C24 121.2(5) . . ?
Na1 O150 H15A 127(3) . . ?
Na1 O150 H15B 132(3) . . ?
H15A O150 H15B 97(4) . . ?
C30 C31 H31 119.9 . . ?
C32 C31 C30 120.2(5) . . ?
C32 C31 H31 119.9 . . ?
H12A N12 H12B 120.0 . . ?
C20 N12 H12A 120.0 . . ?
C20 N12 H12B 120.0 . . ?
O7 C40 C41 118.9(4) . . ?
O8 C40 O7 123.0(5) . . ?
O8 C40 C41 118.1(5) . . ?
C23 C24 C27 120.7(4) . . ?
C23 C24 C25 118.0(5) . . ?
C25 C24 C27 121.4(6) . . ?
C22 C21 C20 121.0(6) . . ?
C26 C21 C22 118.9(5) . . ?
C26 C21 C20 120.1(5) . . ?
C21 C22 H22 120.1 . . ?
C23 C22 C21 119.8(6) . . ?
C23 C22 H22 120.1 . . ?
C27 C32 H32 119.0 . . ?
C31 C32 C27 122.0(4) . . ?
C31 C32 H32 119.0 . . ?
C24 C23 H23 119.0 . . ?
C22 C23 C24 121.9(5) . . ?
C22 C23 H23 119.0 . . ?
C21 C26 H26 119.0 . . ?
C21 C26 C25 121.9(5) . . ?
C25 C26 H26 119.0 . . ?
C24 C25 C26 119.4(6) . . ?
C24 C25 H25 120.3 . . ?
C26 C25 H25 120.3 . . ?
H11C O110 H11D 104.5 . . ?
C27 C28 H28 119.6 . . ?
C29 C28 C27 120.8(5) . . ?
C29 C28 H28 119.6 . . ?
C30 C29 C28 121.9(5) . . ?
C30 C29 H29 119.0 . . ?
C28 C29 H29 119.0 . . ?
C44 B1 C65 115.4(3) . . ?
C44 B1 C58 107.9(4) . . ?
C44 B1 C51 104.6(3) . . ?
C65 B1 C58 108.4(3) . . ?
C65 B1 C51 108.6(4) . . ?
C51 B1 C58 112.0(3) . . ?
N13 C20 N12 119.5(5) . . ?
N13 C20 C21 121.2(5) . . ?
N12 C20 C21 119.3(6) . . ?
Na1 O160 H16A 98.9 . . ?
Na1 O160 H16B 98.8 . . ?
H16A O160 H16B 104.5 . . ?
H13C O130 H13D 97(4) . . ?
H9A O9 H9B 104.5 . . ?
H10E O10 H10F 104.5 . . ?
H11E O11 H11F 104.5 . . ?
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
Na1 O180 2.361(4) . ?
Na1 O190 2.385(5) . ?
Na1 O170 2.521(5) . ?
Na1 O140 2.517(5) . ?
Na1 O100 2.670(9) 1_665 ?
Na1 O150 2.362(5) . ?
Na1 O160 2.183(13) . ?
Na1 H16A 2.4723 . ?
Na1 H16B 2.4705 . ?
O5 C47 1.260(5) . ?
O4 C54 1.258(5) . ?
O6 C47 1.259(5) . ?
O120 H12C 0.8701 . ?
O120 H12D 0.8696 . ?
O3 C54 1.269(6) . ?
O200 H20A 0.8694 . ?
O200 H20B 0.8698 . ?
O2 C61 1.262(6) . ?
O7 C40 1.254(6) . ?
O1 C61 1.259(6) . ?
O180 H18A 0.8759 . ?
O180 H18B 0.8756 . ?
N4 H4A 0.8800 . ?
N4 H4B 0.8800 . ?
N4 C15 1.310(6) . ?
O190 H19A 0.8943 . ?
O190 H19B 0.8930 . ?
N3 H3A 0.8800 . ?
N3 H3B 0.8800 . ?
N3 C15 1.321(6) . ?
O8 C40 1.252(6) . ?
O170 H17A 0.8741 . ?
O170 H17B 0.8745 . ?
N11 H11A 0.8800 . ?
N11 H11B 0.8800 . ?
N11 C33 1.318(6) . ?
N1 H1A 0.8800 . ?
N1 H1B 0.8800 . ?
N1 C1 1.305(6) . ?
N10 H10A 0.8800 . ?
N10 H10B 0.8800 . ?
N10 C33 1.304(7) . ?
N2 H2A 0.8800 . ?
N2 H2B 0.8800 . ?
N2 C1 1.303(6) . ?
O140 H14A 0.90(2) . ?
O140 H14B 0.91(2) . ?
C44 C43 1.406(6) . ?
C44 C45 1.400(6) . ?
C44 B1 1.637(7) . ?
C53 H53 0.9500 . ?
C53 C52 1.376(6) . ?
C53 C48 1.393(6) . ?
C52 H52 0.9500 . ?
C52 C51 1.399(6) . ?
C65 C64 1.407(6) . ?
C65 C66 1.401(6) . ?
C65 B1 1.641(6) . ?
C48 C47 1.504(6) . ?
C48 C49 1.393(6) . ?
C5 C8 1.490(6) . ?
C5 C6 1.396(6) . ?
C5 C4 1.381(6) . ?
C58 C59 1.393(6) . ?
C58 C57 1.414(6) . ?
C58 B1 1.660(6) . ?
C43 H43 0.9500 . ?
C43 C42 1.374(6) . ?
N13 H13A 0.8800 . ?
N13 H13B 0.8800 . ?
N13 C20 1.291(8) . ?
C50 H50 0.9500 . ?
C50 C51 1.408(6) . ?
C50 C49 1.375(6) . ?
C59 H59 0.9500 . ?
C59 C60 1.384(6) . ?
C56 H56 0.9500 . ?
C56 C57 1.384(6) . ?
C56 C55 1.396(6) . ?
C2 C7 1.397(6) . ?
C2 C1 1.485(6) . ?
C2 C3 1.383(7) . ?
C11 C15 1.480(6) . ?
C11 C12 1.389(7) . ?
C11 C10 1.389(6) . ?
C57 H57 0.9500 . ?
C8 C9 1.393(7) . ?
C8 C14 1.386(6) . ?
C62 C67 1.391(6) . ?
C62 C63 1.392(7) . ?
C62 C61 1.512(7) . ?
C7 H7 0.9500 . ?
C7 C6 1.383(6) . ?
C51 B1 1.650(6) . ?
C6 H6 0.9500 . ?
C64 H64 0.9500 . ?
C64 C63 1.392(6) . ?
C55 C54 1.507(6) . ?
C55 C60 1.397(6) . ?
C9 H9 0.9500 . ?
C9 C10 1.388(6) . ?
O100 H10C 1.0040 . ?
O100 H10D 0.9944 . ?
C49 H49 0.9500 . ?
C41 C42 1.400(6) . ?
C41 C46 1.384(7) . ?
C41 C40 1.511(7) . ?
C42 H42 0.9500 . ?
C67 H67 0.9500 . ?
C67 C66 1.394(6) . ?
C12 H12 0.9500 . ?
C12 C14 1.391(7) . ?
C10 H10 0.9500 . ?
C45 H45 0.9500 . ?
C45 C46 1.389(7) . ?
C30 C33 1.490(7) . ?
C30 C31 1.398(7) . ?
C30 C29 1.367(8) . ?
C14 H14 0.9500 . ?
C63 H63 0.9500 . ?
C66 H66 0.9500 . ?
C60 H60 0.9500 . ?
C3 H3 0.9500 . ?
C3 C4 1.384(7) . ?
C4 H4 0.9500 . ?
C46 H46 0.9500 . ?
C27 C24 1.485(7) . ?
C27 C32 1.387(8) . ?
C27 C28 1.398(7) . ?
O150 H15A 0.89(2) . ?
O150 H15B 0.87(2) . ?
C31 H31 0.9500 . ?
C31 C32 1.384(7) . ?
N12 H12A 0.8800 . ?
N12 H12B 0.8800 . ?
N12 C20 1.319(7) . ?
C24 C23 1.393(8) . ?
C24 C25 1.403(7) . ?
C21 C22 1.393(7) . ?
C21 C26 1.371(9) . ?
C21 C20 1.475(8) . ?
C22 H22 0.9500 . ?
C22 C23 1.390(8) . ?
C32 H32 0.9500 . ?
C23 H23 0.9500 . ?
C26 H26 0.9500 . ?
C26 C25 1.404(8) . ?
C25 H25 0.9500 . ?
O110 H11C 0.8705 . ?
O110 H11D 0.8698 . ?
C28 H28 0.9500 . ?
C28 C29 1.382(8) . ?
C29 H29 0.9500 . ?
O160 H16A 0.8701 . ?
O160 H16B 0.8702 . ?
O130 H13C 0.86(2) . ?
O130 H13D 0.89(2) . ?
O9 H9A 0.8704 . ?
O9 H9B 0.8690 . ?
O10 H10E 0.8703 . ?
O10 H10F 0.8694 . ?
O11 H11E 0.8699 . ?
O11 H11F 0.8695 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C44 C43 C42 C41 1.1(7) . . . . ?
C44 C45 C46 C41 0.9(7) . . . . ?
C53 C52 C51 C50 2.4(6) . . . . ?
C53 C52 C51 B1 -179.1(4) . . . . ?
C53 C48 C47 O5 -24.1(6) . . . . ?
C53 C48 C47 O6 155.9(4) . . . . ?
C53 C48 C49 C50 2.4(7) . . . . ?
C52 C53 C48 C47 179.7(4) . . . . ?
C52 C53 C48 C49 -1.4(6) . . . . ?
C52 C51 B1 C44 151.5(4) . . . . ?
C52 C51 B1 C65 -84.8(5) . . . . ?
C52 C51 B1 C58 34.9(6) . . . . ?
C65 C64 C63 C62 1.6(7) . . . . ?
C48 C53 C52 C51 -1.0(7) . . . . ?
C5 C8 C9 C10 -178.9(4) . . . . ?
C5 C8 C14 C12 177.5(4) . . . . ?
C58 C59 C60 C55 -2.4(7) . . . . ?
C43 C44 C45 C46 1.0(6) . . . . ?
C43 C44 B1 C65 170.7(4) . . . . ?
C43 C44 B1 C58 49.4(5) . . . . ?
C43 C44 B1 C51 -70.1(5) . . . . ?
C50 C51 B1 C44 -30.1(5) . . . . ?
C50 C51 B1 C65 93.6(5) . . . . ?
C50 C51 B1 C58 -146.7(4) . . . . ?
C59 C58 C57 C56 -0.1(6) . . . . ?
C59 C58 B1 C44 85.3(5) . . . . ?
C59 C58 B1 C65 -40.2(5) . . . . ?
C59 C58 B1 C51 -160.0(4) . . . . ?
C56 C55 C54 O4 -10.4(7) . . . . ?
C56 C55 C54 O3 169.0(4) . . . . ?
C56 C55 C60 C59 0.2(7) . . . . ?
C2 C7 C6 C5 2.0(7) . . . . ?
C2 C3 C4 C5 1.0(7) . . . . ?
C11 C12 C14 C8 1.5(7) . . . . ?
C57 C58 C59 C60 2.3(7) . . . . ?
C57 C58 B1 C44 -90.1(5) . . . . ?
C57 C58 B1 C65 144.3(4) . . . . ?
C57 C58 B1 C51 24.5(6) . . . . ?
C57 C56 C55 C54 -174.4(4) . . . . ?
C57 C56 C55 C60 1.9(7) . . . . ?
C8 C5 C6 C7 179.5(4) . . . . ?
C8 C5 C4 C3 179.0(4) . . . . ?
C8 C9 C10 C11 1.3(7) . . . . ?
C62 C67 C66 C65 1.5(7) . . . . ?
C7 C2 C1 N1 162.1(4) . . . . ?
C7 C2 C1 N2 -18.6(6) . . . . ?
C7 C2 C3 C4 0.5(7) . . . . ?
C51 C50 C49 C48 -0.9(7) . . . . ?
C6 C5 C8 C9 -139.0(5) . . . . ?
C6 C5 C8 C14 42.4(6) . . . . ?
C6 C5 C4 C3 -1.0(7) . . . . ?
C64 C65 C66 C67 -0.6(6) . . . . ?
C64 C65 B1 C44 -33.9(6) . . . . ?
C64 C65 B1 C58 87.1(5) . . . . ?
C64 C65 B1 C51 -150.9(4) . . . . ?
C55 C56 C57 C58 -2.0(7) . . . . ?
C15 C11 C12 C14 -179.4(4) . . . . ?
C15 C11 C10 C9 178.0(4) . . . . ?
C47 C48 C49 C50 -178.7(4) . . . . ?
C9 C8 C14 C12 -1.2(7) . . . . ?
C54 C55 C60 C59 176.5(4) . . . . ?
C1 C2 C7 C6 177.6(4) . . . . ?
C1 C2 C3 C4 -179.1(4) . . . . ?
C49 C48 C47 O5 157.0(4) . . . . ?
C49 C48 C47 O6 -22.9(7) . . . . ?
C49 C50 C51 C52 -1.4(7) . . . . ?
C49 C50 C51 B1 -179.9(4) . . . . ?
C42 C41 C46 C45 -1.9(7) . . . . ?
C42 C41 C40 O7 10.3(7) . . . . ?
C42 C41 C40 O8 -168.9(5) . . . . ?
C67 C62 C63 C64 -0.7(6) . . . . ?
C67 C62 C61 O2 15.4(6) . . . . ?
C67 C62 C61 O1 -164.4(4) . . . . ?
C12 C11 C15 N4 -19.7(7) . . . . ?
C12 C11 C15 N3 160.2(4) . . . . ?
C12 C11 C10 C9 -1.0(7) . . . . ?
C10 C11 C15 N4 161.4(4) . . . . ?
C10 C11 C15 N3 -18.8(7) . . . . ?
C10 C11 C12 C14 -0.4(7) . . . . ?
C45 C44 C43 C42 -2.0(6) . . . . ?
C45 C44 B1 C65 -20.4(6) . . . . ?
C45 C44 B1 C58 -141.7(4) . . . . ?
C45 C44 B1 C51 98.8(5) . . . . ?
C30 C31 C32 C27 -0.1(8) . . . . ?
C14 C8 C9 C10 -0.2(7) . . . . ?
C63 C62 C67 C66 -0.8(6) . . . . ?
C63 C62 C61 O2 -163.1(4) . . . . ?
C63 C62 C61 O1 17.0(7) . . . . ?
C66 C65 C64 C63 -0.9(6) . . . . ?
C66 C65 B1 C44 149.6(4) . . . . ?
C66 C65 B1 C58 -89.4(4) . . . . ?
C66 C65 B1 C51 32.6(5) . . . . ?
C60 C55 C54 O4 173.4(5) . . . . ?
C60 C55 C54 O3 -7.2(7) . . . . ?
C33 C30 C31 C32 178.1(4) . . . . ?
C33 C30 C29 C28 -177.6(5) . . . . ?
C3 C2 C7 C6 -2.0(7) . . . . ?
C3 C2 C1 N1 -18.4(6) . . . . ?
C3 C2 C1 N2 160.9(5) . . . . ?
C4 C5 C8 C9 41.0(6) . . . . ?
C4 C5 C8 C14 -137.7(5) . . . . ?
C4 C5 C6 C7 -0.5(7) . . . . ?
C61 C62 C67 C66 -179.4(4) . . . . ?
C61 C62 C63 C64 177.9(4) . . . . ?
C46 C41 C42 C43 0.9(6) . . . . ?
C46 C41 C40 O7 -169.1(5) . . . . ?
C46 C41 C40 O8 11.8(7) . . . . ?
C27 C24 C23 C22 -179.0(4) . . . . ?
C27 C24 C25 C26 179.4(4) . . . . ?
C27 C28 C29 C30 -1.0(10) . . . . ?
C31 C30 C33 N11 -169.5(4) . . . . ?
C31 C30 C33 N10 8.9(7) . . . . ?
C31 C30 C29 C28 3.1(9) . . . . ?
C40 C41 C42 C43 -178.5(4) . . . . ?
C40 C41 C46 C45 177.5(4) . . . . ?
C24 C27 C32 C31 -177.8(5) . . . . ?
C24 C27 C28 C29 178.3(5) . . . . ?
C21 C22 C23 C24 0.0(7) . . . . ?
C21 C26 C25 C24 -0.6(7) . . . . ?
C22 C21 C26 C25 0.9(8) . . . . ?
C22 C21 C20 N13 31.8(8) . . . . ?
C22 C21 C20 N12 -148.3(6) . . . . ?
C32 C27 C24 C23 147.2(5) . . . . ?
C32 C27 C24 C25 -32.1(7) . . . . ?
C32 C27 C28 C29 -1.7(9) . . . . ?
C23 C24 C25 C26 0.0(7) . . . . ?
C26 C21 C22 C23 -0.6(7) . . . . ?
C26 C21 C20 N13 -147.3(6) . . . . ?
C26 C21 C20 N12 32.7(8) . . . . ?
C25 C24 C23 C22 0.3(7) . . . . ?
C28 C27 C24 C23 -32.8(7) . . . . ?
C28 C27 C24 C25 147.8(5) . . . . ?
C28 C27 C32 C31 2.2(8) . . . . ?
C29 C30 C33 N11 11.3(7) . . . . ?
C29 C30 C33 N10 -170.4(5) . . . . ?
C29 C30 C31 C32 -2.6(8) . . . . ?
B1 C44 C43 C42 168.1(4) . . . . ?
B1 C44 C45 C46 -168.4(4) . . . . ?
B1 C65 C64 C63 -177.6(4) . . . . ?
B1 C65 C66 C67 176.3(4) . . . . ?
B1 C58 C59 C60 -173.6(4) . . . . ?
B1 C58 C57 C56 175.6(4) . . . . ?
C20 C21 C22 C23 -179.7(5) . . . . ?
C20 C21 C26 C25 180.0(5) . . . . ?
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-5.4115 -0.2236 11.8496 0.1643 0.6944 0.7006
5.9973 -0.2373 -11.5721 -0.1756 -0.7411 -0.6480
-5.2322 -8.5250 2.6595 -0.8282 0.1992 0.5238
6.1529 0.2631 10.8379 0.5656 -0.1331 0.8139
-5.6498 0.5753 -11.1204 -0.4852 0.1137 -0.8670
-6.4487 -0.8081 -10.5975 -0.6150 0.1450 -0.7750
4.8417 8.5278 -3.3753 0.7931 -0.1910 -0.5783
