# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
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data_Bibrocathol-1-Monoclinic
_database_code_depnum_ccdc_archive 'CCDC 2190211'
loop_
_audit_author_name
_audit_author_address
'Erik Svensson Grape'
;Stockholm University
Sweden
;
_audit_update_record             
;
2022-08-17 deposited with the CCDC.	2022-08-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C60 Bi10 Br40 O25'
_chemical_formula_weight         6406.59

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Bi Bi 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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.
;

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'

_cell_length_a                   17.01(9)
_cell_length_b                   27.26(14)
_cell_length_c                   26.21(13)
_cell_angle_alpha                90
_cell_angle_beta                 94.7(2)
_cell_angle_gamma                90
_cell_volume                     12113(105)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    120385
_cell_measurement_theta_min      0.050
_cell_measurement_theta_max      0.841

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.513
_exptl_crystal_F_000             2453
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    0.000
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.0251
_diffrn_radiation_type           electron
_diffrn_source                   ?
_diffrn_measurement_device_type  'JEOL JEM-2100 LaB6'
_diffrn_measurement_method       'continuous rotation'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            120385
_diffrn_reflns_av_unetI/netI     0.2244
_diffrn_reflns_av_R_equivalents  0.2785
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         0.050
_diffrn_reflns_theta_max         0.841
_diffrn_reflns_theta_full        0.841
_diffrn_measured_fraction_theta_max 0.898
_diffrn_measured_fraction_theta_full 0.898
_diffrn_reflns_Laue_measured_fraction_max 0.898
_diffrn_reflns_Laue_measured_fraction_full 0.898
_diffrn_reflns_point_group_measured_fraction_max 0.898
_diffrn_reflns_point_group_measured_fraction_full 0.898
_reflns_number_total             18190
_reflns_number_gt                10695
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       
;
Stef Smeets, Bin Wang, Magdalena O. Cichocka, Jonas Angstrom, Wei Wan.
(2018, April 11). Instamatic (Version 0.6). Zenodo.
http://doi.org/10.5281/zenodo.1217026
;
_computing_cell_refinement       
;
Kabsch, W. (2010). XDS. Acta Crystallographica Section D:
Biological Crystallography, 66(2), 125-132.
;
_computing_data_reduction        
;
Kabsch, W. (2010). XDS. Acta Crystallographica Section D:
Biological Crystallography, 66(2), 125-132.
;
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1850P)²+54.7346P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         18190
_refine_ls_number_parameters     481
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.2979
_refine_ls_R_factor_gt           0.2346
_refine_ls_wR_factor_ref         0.5555
_refine_ls_wR_factor_gt          0.5186
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_restrained_S_all      1.114
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Bi6 Bi 0.8405(3) 0.33596(15) 0.28957(16) 0.0455(10) Uiso 1 1 d . . . . .
O22 O 0.747(2) 0.5051(13) 0.2552(14) 0.099(10) Uiso 1 1 d . U . . .
Bi4 Bi 0.7328(3) 0.43698(15) 0.19599(16) 0.0480(11) Uiso 1 1 d . U . . .
O25 O 0.722(3) 0.2077(14) 0.2302(15) 0.102(11) Uiso 1 1 d . . . . .
Bi3 Bi 0.8359(3) 0.48310(16) 0.31759(17) 0.0527(11) Uiso 1 1 d . U . . .
Bi9 Bi 0.8492(3) 0.19066(15) 0.24592(16) 0.0497(11) Uiso 1 1 d . . . . .
Bi2 Bi 0.6404(3) 0.54560(15) 0.29220(17) 0.0503(11) Uiso 1 1 d . U . . .
Bi1 Bi 0.7868(3) 0.58099(15) 0.19364(16) 0.0474(11) Uiso 1 1 d . U . . .
Bi10 Bi 0.6717(3) 0.13762(16) 0.17577(17) 0.0528(11) Uiso 1 1 d . . . . .
O21 O 0.719(2) 0.6011(13) 0.2696(14) 0.098(10) Uiso 1 1 d . U . . .
Bi7 Bi 0.6914(3) 0.28804(16) 0.18514(18) 0.0561(12) Uiso 1 1 d . . . . .
Bi5 Bi 0.6395(3) 0.38931(17) 0.31400(19) 0.0605(13) Uiso 1 1 d . U . . .
Bi8 Bi 0.6623(3) 0.23507(17) 0.31234(19) 0.0611(13) Uiso 1 1 d . . . . .
Br16 Br 1.0304(7) 0.3664(4) 0.2440(4) 0.069(3) Uiso 1 1 d . . . . .
Br28 Br 0.9948(6) 0.2347(3) 0.1649(3) 0.056(2) Uiso 1 1 d . . . . .
Br21 Br 0.6723(7) 0.2774(4) 0.4522(4) 0.072(3) Uiso 1 1 d . . . . .
Br17 Br 0.4205(7) 0.5316(4) 0.2929(4) 0.074(3) Uiso 1 1 d . . . . .
Br6 Br 0.3774(7) 0.6605(4) 0.0867(4) 0.081(3) Uiso 1 1 d . . . . .
Br8 Br 0.6108(7) 0.4979(4) 0.0896(4) 0.071(3) Uiso 1 1 d . . . . .
Br18 Br 0.3157(7) 0.5262(4) 0.1736(4) 0.080(3) Uiso 1 1 d . . . . .
Br20 Br 0.5130(7) 0.3558(4) 0.1225(4) 0.079(3) Uiso 1 1 d . . . . .
Br1 Br 1.0160(8) 0.6965(4) 0.1299(5) 0.092(4) Uiso 1 1 d . . . . .
Br24 Br 0.9468(6) 0.4583(3) 0.4432(4) 0.063(2) Uiso 1 1 d . . . . .
Br29 Br 0.4356(8) 0.3694(4) 0.3457(4) 0.086(3) Uiso 1 1 d . . . . .
Br26 Br 0.9730(8) 0.3913(4) 0.0080(4) 0.086(3) Uiso 1 1 d . . . . .
Br13 Br 0.9156(7) 0.5495(4) 0.0824(4) 0.077(3) Uiso 1 1 d . . . . .
Br36 Br 1.0155(7) 0.3065(4) 0.3831(4) 0.074(3) Uiso 1 1 d . . . . .
Br22 Br 0.7274(8) 0.3394(5) 0.5633(5) 0.098(4) Uiso 1 1 d . . . . .
Br37 Br 0.6797(8) 0.2849(4) 0.0391(5) 0.089(3) Uiso 1 1 d . . . . .
Br12 Br 0.8808(8) 0.6192(4) 0.4659(5) 0.093(4) Uiso 1 1 d . . . . .
Br25 Br 0.7870(7) 0.4202(4) 0.0485(4) 0.074(3) Uiso 1 1 d . . . . .
Br5 Br 0.4239(7) 0.6781(4) 0.2159(4) 0.072(3) Uiso 1 1 d . . . . .
Br35 Br 0.9792(8) 0.2789(4) 0.5096(5) 0.092(4) Uiso 1 1 d . . . . .
Br19 Br 0.3626(9) 0.4351(5) 0.0889(5) 0.100(4) Uiso 1 1 d . . . . .
Br9 Br 0.6057(8) 0.4380(4) 0.4487(4) 0.086(3) Uiso 1 1 d . . . . .
Br33 Br 0.7604(7) 0.1252(4) 0.4333(4) 0.084(3) Uiso 1 1 d . . . . .
Br7 Br 0.4794(9) 0.5733(5) 0.0214(5) 0.102(4) Uiso 1 1 d . . . . .
Br40 Br 0.9452(8) 0.1014(4) 0.0877(4) 0.088(3) Uiso 1 1 d . . . . .
Br14 Br 1.1105(9) 0.5084(5) 0.0836(5) 0.104(4) Uiso 1 1 d . . . . .
Br39 Br 0.9703(11) 0.1761(6) -0.0160(6) 0.128(5) Uiso 1 1 d . . . . .
Br27 Br 1.0804(8) 0.2969(4) 0.0639(5) 0.094(4) Uiso 1 1 d . . . . .
Br32 Br 0.4476(8) 0.1955(4) 0.1571(4) 0.087(3) Uiso 1 1 d . . . . .
Br15 Br 1.1637(9) 0.4119(5) 0.1621(5) 0.107(4) Uiso 1 1 d . . . . .
Br23 Br 0.8725(8) 0.4271(4) 0.5611(5) 0.089(3) Uiso 1 1 d . . . . .
Br38 Br 0.8304(10) 0.2671(5) -0.0456(6) 0.120(5) Uiso 1 1 d . . . . .
Br4 Br 1.0465(9) 0.5201(5) 0.3109(5) 0.101(4) Uiso 1 1 d . . . . .
Br11 Br 0.7679(11) 0.5981(6) 0.5701(6) 0.129(5) Uiso 1 1 d . . . . .
Br34 Br 0.8394(8) 0.1962(4) 0.5354(5) 0.091(3) Uiso 1 1 d . . . . .
Br31 Br 0.2732(11) 0.2610(6) 0.1731(6) 0.128(5) Uiso 1 1 d . . . . .
Br30 Br 0.2671(13) 0.3452(7) 0.2708(7) 0.153(6) Uiso 1 1 d . . . . .
Br10 Br 0.6270(10) 0.5051(5) 0.5615(6) 0.118(5) Uiso 1 1 d . . . . .
Br2 Br 1.1993(10) 0.6672(6) 0.1860(6) 0.125(5) Uiso 1 1 d . . . . .
Br3 Br 1.2113(11) 0.5828(6) 0.2842(6) 0.131(5) Uiso 1 1 d . . . . .
O3 O 0.6249(15) 0.5338(8) 0.2079(9) 0.046(6) Uiso 1 1 d . . . . .
O6 O 0.7266(17) 0.4748(9) 0.3671(10) 0.059(7) Uiso 1 1 d . . . . .
O13 O 0.8300(17) 0.2796(10) 0.1852(10) 0.061(7) Uiso 1 1 d . . . . .
C58 C 0.818(2) 0.2270(12) 0.0154(13) 0.073(10) Uiso 1 1 d . . . . .
C46 C 0.363(3) 0.3111(15) 0.2619(16) 0.099(13) Uiso 1 1 d . . . . .
O2 O 0.8969(16) 0.5662(8) 0.2494(9) 0.050(6) Uiso 1 1 d . . . . .
C49 C 0.8982(15) 0.2308(8) 0.3569(9) 0.036(6) Uiso 1 1 d . . . . .
C8 C 0.5344(13) 0.5964(7) 0.2026(5) 0.067(9) Uiso 1 1 d G . . . .
C7 C 0.5688(11) 0.5582(6) 0.1772(7) 0.040(6) Uiso 1 1 d G . . . .
C12 C 0.5486(13) 0.5506(7) 0.1253(7) 0.067(9) Uiso 1 1 d G . . . .
C11 C 0.4940(14) 0.5812(8) 0.0989(5) 0.067(9) Uiso 1 1 d G . . . .
C10 C 0.4597(13) 0.6194(7) 0.1243(8) 0.088(11) Uiso 1 1 d G . . . .
C9 C 0.4799(13) 0.6270(7) 0.1761(8) 0.057(8) Uiso 1 1 d G . . . .
C57 C 0.761(2) 0.2341(10) 0.0526(11) 0.057(8) Uiso 1 1 d . . . . .
O12 O 0.7604(16) 0.3170(9) 0.3595(10) 0.054(6) Uiso 1 1 d . . . . .
C24 C 0.9986(17) 0.4187(9) 0.1983(10) 0.045(7) Uiso 1 1 d . . . . .
C38 C 0.8245(9) 0.3435(7) 0.1234(7) 0.077(10) Uiso 1 1 d G . . . .
C37 C 0.8656(11) 0.3044(6) 0.1469(6) 0.045(7) Uiso 1 1 d G . . . .
C42 C 0.9376(11) 0.2900(5) 0.1303(7) 0.053(7) Uiso 1 1 d G . . . .
C41 C 0.9686(9) 0.3148(7) 0.0901(7) 0.062(8) Uiso 1 1 d G . . . .
C40 C 0.9276(11) 0.3539(6) 0.0665(6) 0.060(8) Uiso 1 1 d G . . . .
C39 C 0.8555(11) 0.3682(5) 0.0832(7) 0.039(6) Uiso 1 1 d G . . . .
C25 C 0.532(2) 0.4127(13) 0.2171(14) 0.078(10) Uiso 1 1 d . . . . .
C43 C 0.510(3) 0.2546(13) 0.2473(14) 0.083(11) Uiso 1 1 d . . . . .
C21 C 0.955(2) 0.4977(13) 0.1247(13) 0.077(10) Uiso 1 1 d . . . . .
O14 O 0.7514(18) 0.3560(10) 0.1474(11) 0.064(7) Uiso 1 1 d . . . . .
O19 O 0.8021(17) 0.1330(9) 0.1427(10) 0.060(7) Uiso 1 1 d . U . . .
O7 O 0.8661(15) 0.4188(8) 0.2231(9) 0.045(6) Uiso 1 1 d . . . . .
O9 O 0.5921(18) 0.3816(10) 0.2291(10) 0.062(7) Uiso 1 1 d . . . . .
C47 C 0.371(3) 0.2807(18) 0.2170(19) 0.120(16) Uiso 1 1 d . . . . .
O10 O 0.565(2) 0.4592(11) 0.2926(12) 0.076(8) Uiso 1 1 d . . . . .
C55 C 0.809(2) 0.1623(12) 0.1043(13) 0.068(9) Uiso 1 1 d . . . . .
C19 C 0.919(3) 0.4358(14) 0.1942(15) 0.087(11) Uiso 1 1 d . . . . .
C54 C 0.943(2) 0.2555(12) 0.4000(13) 0.073(10) Uiso 1 1 d . . . . .
O8 O 0.8199(17) 0.4933(9) 0.1648(10) 0.060(7) Uiso 1 1 d . . . . .
C30 C 0.4852(16) 0.4084(8) 0.1674(9) 0.036(6) Uiso 1 1 d . . . . .
C20 C 0.8989(18) 0.4767(10) 0.1605(11) 0.052(7) Uiso 1 1 d . . . . .
C23 C 1.0612(18) 0.4358(10) 0.1650(10) 0.049(7) Uiso 1 1 d . . . . .
O16 O 0.574(2) 0.3009(11) 0.3224(11) 0.073(8) Uiso 1 1 d . . . . .
O1 O 0.8820(18) 0.6392(10) 0.1874(11) 0.065(7) Uiso 1 1 d . . . . .
C50 C 0.8433(18) 0.1913(10) 0.3699(11) 0.051(7) Uiso 1 1 d . . . . .
O11 O 0.869(2) 0.3940(11) 0.3531(12) 0.075(8) Uiso 1 1 d . . . . .
C56 C 0.752(2) 0.2030(13) 0.0945(14) 0.078(10) Uiso 1 1 d . . . . .
C14 C 0.7280(15) 0.5019(8) 0.4143(7) 0.067(9) Uiso 1 1 d G . . . .
C15 C 0.6847(13) 0.4915(8) 0.4557(9) 0.091(12) Uiso 1 1 d G . . . .
C16 C 0.6963(15) 0.5189(9) 0.5004(8) 0.080(10) Uiso 1 1 d G . . . .
C17 C 0.7512(16) 0.5567(9) 0.5037(8) 0.087(11) Uiso 1 1 d G . . . .
C18 C 0.7945(15) 0.5672(8) 0.4623(10) 0.118(15) Uiso 1 1 d G . . . .
C13 C 0.7829(14) 0.5398(9) 0.4176(8) 0.075(10) Uiso 1 1 d G . . . .
C26 C 0.5139(18) 0.4531(10) 0.2513(10) 0.048(7) Uiso 1 1 d . . . . .
C22 C 1.031(2) 0.4779(12) 0.1263(13) 0.075(10) Uiso 1 1 d . . . . .
C48 C 0.434(2) 0.2484(11) 0.2143(12) 0.063(9) Uiso 1 1 d . . . . .
O18 O 0.8104(15) 0.1678(8) 0.3256(9) 0.046(6) Uiso 1 1 d . . . . .
C45 C 0.436(2) 0.3196(12) 0.2931(13) 0.071(9) Uiso 1 1 d . . . . .
O20 O 0.684(3) 0.2132(14) 0.1268(15) 0.104(11) Uiso 1 1 d . U . . .
C60 C 0.872(2) 0.1574(13) 0.0713(14) 0.078(10) Uiso 1 1 d . . . . .
O17 O 0.8986(18) 0.2460(10) 0.3062(10) 0.063(7) Uiso 1 1 d . . . . .
C53 C 0.9277(19) 0.2426(10) 0.4528(11) 0.055(8) Uiso 1 1 d . . . . .
C31 C 0.8365(14) 0.3799(8) 0.4055(6) 0.077(10) Uiso 1 1 d G . . . .
C36 C 0.8645(12) 0.4032(7) 0.4506(8) 0.103(13) Uiso 1 1 d G . . . .
C35 C 0.8362(13) 0.3895(7) 0.4968(6) 0.050(7) Uiso 1 1 d G . . . .
C34 C 0.7800(13) 0.3525(8) 0.4979(6) 0.070(9) Uiso 1 1 d G . . . .
C33 C 0.7520(12) 0.3293(7) 0.4528(8) 0.065(9) Uiso 1 1 d G . . . .
C32 C 0.7803(13) 0.3430(7) 0.4066(6) 0.051(7) Uiso 1 1 d G . . . .
C27 C 0.442(2) 0.4830(13) 0.2402(14) 0.086(11) Uiso 1 1 d . . . . .
O4 O 0.563(2) 0.6102(11) 0.2546(12) 0.076(8) Uiso 1 1 d . . . . .
C28 C 0.400(2) 0.4797(11) 0.1910(12) 0.061(8) Uiso 1 1 d . . . . .
C44 C 0.503(2) 0.2925(13) 0.2859(14) 0.079(10) Uiso 1 1 d . . . . .
O5 O 0.835(2) 0.5526(13) 0.3771(14) 0.096(10) Uiso 1 1 d . . . . .
C51 C 0.8308(18) 0.1779(10) 0.4206(11) 0.051(7) Uiso 1 1 d . . . . .
C1 C 0.9613(12) 0.6229(8) 0.2005(9) 0.081(11) Uiso 1 1 d G . . . .
C6 C 0.9659(12) 0.5867(8) 0.2380(9) 0.084(11) Uiso 1 1 d G . . . .
C5 C 1.0389(15) 0.5723(7) 0.2607(7) 0.070(9) Uiso 1 1 d G . . . .
C4 C 1.1074(12) 0.5941(9) 0.2459(9) 0.076(9) Uiso 1 1 d G U . . .
C3 C 1.1028(12) 0.6302(9) 0.2084(9) 0.116(13) Uiso 1 1 d G U . . .
C2 C 1.0298(15) 0.6446(7) 0.1857(8) 0.061(8) Uiso 1 1 d G U . . .
O15 O 0.583(2) 0.2267(13) 0.2428(14) 0.096(10) Uiso 1 1 d . . . . .
O24 O 0.715(2) 0.2995(12) 0.2658(13) 0.083(9) Uiso 1 1 d . . . . .
C29 C 0.430(3) 0.4432(15) 0.1535(16) 0.096(12) Uiso 1 1 d . . . . .
C59 C 0.885(2) 0.1845(13) 0.0312(14) 0.083(11) Uiso 1 1 d . . . . .
C52 C 0.863(2) 0.2092(13) 0.4638(14) 0.083(11) Uiso 1 1 d . . . . .
O23 O 0.754(2) 0.4047(12) 0.2813(13) 0.088(9) Uiso 1 1 d . U . . .

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Bi6 O11 2.32(3) . ?
Bi6 O23 2.38(4) . ?
Bi6 O24 2.39(4) . ?
Bi6 O12 2.43(3) . ?
Bi6 O17 2.67(3) . ?
O22 Bi3 2.21(4) . ?
O22 Bi2 2.40(4) . ?
O22 Bi4 2.42(4) . ?
Bi4 O8 2.33(3) . ?
Bi4 O7 2.37(3) . ?
Bi4 O23 2.40(4) . ?
Bi4 O14 2.58(3) . ?
O25 Bi9 2.22(4) . ?
O25 Bi10 2.50(4) . ?
O25 Bi7 2.52(4) . ?
O25 Bi8 2.56(4) . ?
Bi3 O6 2.36(3) . ?
Bi3 O5 2.45(4) . ?
Bi3 O11 2.65(3) . ?
Bi3 O23 2.68(4) . ?
Bi9 O17 2.29(3) . ?
Bi9 O18 2.33(3) . ?
Bi9 O4 2.65(3) 2_645 ?
Bi2 O21 2.13(4) . ?
Bi2 O3 2.23(3) . ?
Bi2 O4 2.36(3) . ?
Bi2 O10 2.68(3) . ?
Bi1 O1 2.28(3) . ?
Bi1 O2 2.31(3) . ?
Bi1 O21 2.44(4) . ?
Bi1 O8 2.58(3) . ?
Bi10 O20 2.44(4) . ?
Bi10 O19 2.45(3) . ?
Bi10 O21 2.46(4) 2_645 ?
Bi7 O24 2.14(3) . ?
Bi7 O13 2.37(3) . ?
Bi7 O14 2.37(3) . ?
Bi7 O20 2.55(4) . ?
Bi5 O23 2.23(4) . ?
Bi5 O9 2.31(3) . ?
Bi5 O10 2.33(3) . ?
Bi5 O16 2.67(3) . ?
Bi8 O15 2.19(4) . ?
Bi8 O24 2.36(4) . ?
Bi8 O16 2.37(3) . ?
Br16 C24 1.91(3) . ?
Br28 C42 1.976(16) . ?
Br21 C33 1.960(19) . ?
Br17 C27 1.97(4) . ?
Br6 C10 1.989(18) . ?
Br8 C12 2.055(19) . ?
Br18 C28 1.94(3) . ?
Br20 C30 1.94(3) . ?
Br1 C2 2.03(2) . ?
Br24 C36 2.074(19) . ?
Br29 C45 1.93(4) . ?
Br26 C40 2.05(2) . ?
Br13 C21 1.88(4) . ?
Br36 C54 1.94(4) . ?
Br22 C34 2.03(2) . ?
Br37 C57 1.96(3) . ?
Br12 C18 2.04(2) . ?
Br25 C39 2.005(17) . ?
Br5 C9 2.024(19) . ?
Br35 C53 1.94(3) . ?
Br19 C29 1.98(4) . ?
Br9 C15 1.98(2) . ?
Br33 C51 1.92(3) . ?
Br7 C11 2.04(2) . ?
Br40 C60 1.99(4) . ?
Br14 C22 2.00(4) . ?
Br39 C59 1.99(5) . ?
Br27 C41 2.13(2) . ?
Br32 C48 2.11(3) . ?
Br15 C23 1.87(3) . ?
Br23 C35 2.027(19) . ?
Br38 C58 1.96(4) . ?
Br4 C5 1.94(2) . ?
Br11 C17 2.07(2) . ?
Br34 C52 1.98(4) . ?
Br31 C47 2.02(5) . ?
Br30 C46 1.91(5) . ?
Br10 C16 2.10(3) . ?
Br2 C3 2.05(3) . ?
Br3 C4 1.98(2) . ?
O3 C7 1.37(3) . ?
O6 C14 1.44(3) . ?
O13 C37 1.39(3) . ?
C58 C57 1.45(5) . ?
C58 C59 1.65(5) . ?
C46 C45 1.44(5) . ?
C46 C47 1.45(6) . ?
O2 C6 1.35(3) . ?
C49 O17 1.39(4) . ?
C49 C54 1.47(4) . ?
C49 C50 1.48(4) . ?
C8 C7 1.3900 . ?
C8 C9 1.3900 . ?
C8 O4 1.46(3) . ?
C7 C12 1.3900 . ?
C12 C11 1.3900 . ?
C11 C10 1.3900 . ?
C10 C9 1.3900 . ?
C57 C56 1.40(5) . ?
O12 C32 1.44(3) . ?
C24 C19 1.42(5) . ?
C24 C23 1.50(4) . ?
C38 C37 1.3900 . ?
C38 C39 1.3900 . ?
C38 O14 1.48(3) . ?
C37 C42 1.3900 . ?
C42 C41 1.3900 . ?
C41 C40 1.3900 . ?
C40 C39 1.3900 . ?
C25 O9 1.34(4) . ?
C25 C26 1.47(4) . ?
C25 C30 1.48(4) . ?
C43 C44 1.46(5) . ?
C43 O15 1.46(5) . ?
C43 C48 1.51(5) . ?
C21 C22 1.41(5) . ?
C21 C20 1.50(5) . ?
O19 C55 1.30(4) . ?
O7 C19 1.31(5) . ?
C47 C48 1.39(6) . ?
O10 C26 1.34(4) . ?
C55 C60 1.44(5) . ?
C55 C56 1.48(5) . ?
C19 C20 1.45(4) . ?
C54 C53 1.47(5) . ?
O8 C20 1.43(4) . ?
C30 C29 1.36(5) . ?
C23 C22 1.59(4) . ?
O16 C44 1.49(5) . ?
O1 C1 1.44(3) . ?
C50 O18 1.40(3) . ?
C50 C51 1.41(4) . ?
O11 C31 1.57(4) . ?
C56 O20 1.52(6) . ?
C14 C15 1.3900 . ?
C14 C13 1.3900 . ?
C15 C16 1.3900 . ?
C16 C17 1.3900 . ?
C17 C18 1.3900 . ?
C18 C13 1.3900 . ?
C13 O5 1.48(5) . ?
C26 C27 1.48(5) . ?
C45 C44 1.39(5) . ?
C60 C59 1.32(5) . ?
C53 C52 1.47(5) . ?
C31 C36 1.3900 . ?
C31 C32 1.3900 . ?
C36 C35 1.3900 . ?
C35 C34 1.3900 . ?
C34 C33 1.3900 . ?
C33 C32 1.3900 . ?
C27 C28 1.43(4) . ?
C28 C29 1.51(5) . ?
C51 C52 1.49(4) . ?
C1 C6 1.3900 . ?
C1 C2 1.3900 . ?
C6 C5 1.3900 . ?
C5 C4 1.3900 . ?
C4 C3 1.3900 . ?
C3 C2 1.3900 . ?

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
O11 Bi6 O23 67.9(11) . . ?
O11 Bi6 O24 127.2(13) . . ?
O23 Bi6 O24 76.8(12) . . ?
O11 Bi6 O12 72.7(11) . . ?
O23 Bi6 O12 81.7(11) . . ?
O24 Bi6 O12 64.2(11) . . ?
O11 Bi6 O17 117.1(10) . . ?
O23 Bi6 O17 163.0(12) . . ?
O24 Bi6 O17 88.3(10) . . ?
O12 Bi6 O17 84.5(9) . . ?
Bi3 O22 Bi2 108.6(16) . . ?
Bi3 O22 Bi4 107.1(15) . . ?
Bi2 O22 Bi4 124.8(17) . . ?
O8 Bi4 O7 67.9(9) . . ?
O8 Bi4 O23 121.2(11) . . ?
O7 Bi4 O23 65.0(11) . . ?
O8 Bi4 O22 71.6(12) . . ?
O7 Bi4 O22 85.6(11) . . ?
O23 Bi4 O22 71.6(12) . . ?
O8 Bi4 O14 106.4(10) . . ?
O7 Bi4 O14 79.4(9) . . ?
O23 Bi4 O14 97.5(11) . . ?
O22 Bi4 O14 164.3(11) . . ?
Bi9 O25 Bi10 103.3(16) . . ?
Bi9 O25 Bi7 115.5(17) . . ?
Bi10 O25 Bi7 110.4(14) . . ?
Bi9 O25 Bi8 110.7(15) . . ?
Bi10 O25 Bi8 124.1(18) . . ?
Bi7 O25 Bi8 93.4(14) . . ?
O22 Bi3 O6 85.0(14) . . ?
O22 Bi3 O5 102.9(13) . . ?
O6 Bi3 O5 71.3(12) . . ?
O22 Bi3 O11 128.5(12) . . ?
O6 Bi3 O11 82.9(10) . . ?
O5 Bi3 O11 119.8(11) . . ?
O22 Bi3 O23 69.6(12) . . ?
O6 Bi3 O23 73.1(11) . . ?
O5 Bi3 O23 144.2(14) . . ?
O11 Bi3 O23 59.0(10) . . ?
O25 Bi9 O17 106.7(13) . . ?
O25 Bi9 O18 83.1(12) . . ?
O17 Bi9 O18 70.9(10) . . ?
O25 Bi9 O4 135.4(12) . 2_645 ?
O17 Bi9 O4 112.0(10) . 2_645 ?
O18 Bi9 O4 89.0(9) . 2_645 ?
O21 Bi2 O3 81.6(12) . . ?
O21 Bi2 O4 72.2(14) . . ?
O3 Bi2 O4 71.1(10) . . ?
O21 Bi2 O22 72.6(15) . . ?
O3 Bi2 O22 64.2(11) . . ?
O4 Bi2 O22 126.0(13) . . ?
O21 Bi2 O10 159.1(13) . . ?
O3 Bi2 O10 81.9(9) . . ?
O4 Bi2 O10 114.0(11) . . ?
O22 Bi2 O10 88.7(12) . . ?
O1 Bi1 O2 67.9(10) . . ?
O1 Bi1 O21 106.7(12) . . ?
O2 Bi1 O21 86.3(12) . . ?
O1 Bi1 O8 116.7(11) . . ?
O2 Bi1 O8 80.7(8) . . ?
O21 Bi1 O8 125.1(11) . . ?
O20 Bi10 O19 74.8(12) . . ?
O20 Bi10 O21 123.6(14) . 2_645 ?
O19 Bi10 O21 61.5(12) . 2_645 ?
O20 Bi10 O25 67.3(13) . . ?
O19 Bi10 O25 87.9(12) . . ?
O21 Bi10 O25 76.7(13) 2_645 . ?
Bi2 O21 Bi1 114.5(16) . . ?
Bi2 O21 Bi10 125.9(17) . 2_655 ?
Bi1 O21 Bi10 100.5(16) . 2_655 ?
O24 Bi7 O13 84.6(12) . . ?
O24 Bi7 O14 104.2(11) . . ?
O13 Bi7 O14 67.3(10) . . ?
O24 Bi7 O25 69.5(13) . . ?
O13 Bi7 O25 75.4(12) . . ?
O14 Bi7 O25 142.6(13) . . ?
O24 Bi7 O20 134.8(12) . . ?
O13 Bi7 O20 85.6(12) . . ?
O14 Bi7 O20 112.2(13) . . ?
O25 Bi7 O20 65.4(13) . . ?
O23 Bi5 O9 83.9(12) . . ?
O23 Bi5 O10 103.2(13) . . ?
O9 Bi5 O10 72.7(10) . . ?
O23 Bi5 O16 125.8(12) . . ?
O9 Bi5 O16 83.2(9) . . ?
O10 Bi5 O16 122.2(11) . . ?
O15 Bi8 O24 83.3(13) . . ?
O15 Bi8 O16 79.4(13) . . ?
O24 Bi8 O16 76.5(12) . . ?
O15 Bi8 O25 62.2(15) . . ?
O24 Bi8 O25 65.7(12) . . ?
O16 Bi8 O25 127.7(11) . . ?
C7 O3 Bi2 122.2(17) . . ?
C14 O6 Bi3 117.7(18) . . ?
C37 O13 Bi7 116.4(17) . . ?
C57 C58 C59 114(3) . . ?
C57 C58 Br38 127(2) . . ?
C59 C58 Br38 118(3) . . ?
C45 C46 C47 115(4) . . ?
C45 C46 Br30 123(3) . . ?
C47 C46 Br30 121(3) . . ?
C6 O2 Bi1 117.4(17) . . ?
O17 C49 C54 124(2) . . ?
O17 C49 C50 119(2) . . ?
C54 C49 C50 117(2) . . ?
C7 C8 C9 120.0 . . ?
C7 C8 O4 121.1(18) . . ?
C9 C8 O4 118.2(17) . . ?
O3 C7 C12 127.3(16) . . ?
O3 C7 C8 112.5(16) . . ?
C12 C7 C8 120.0 . . ?
C7 C12 C11 120.0 . . ?
C7 C12 Br8 117.1(11) . . ?
C11 C12 Br8 122.6(11) . . ?
C12 C11 C10 120.0 . . ?
C12 C11 Br7 117.2(12) . . ?
C10 C11 Br7 122.3(12) . . ?
C9 C10 C11 120.0 . . ?
C9 C10 Br6 120.5(12) . . ?
C11 C10 Br6 119.4(12) . . ?
C10 C9 C8 120.0 . . ?
C10 C9 Br5 121.2(11) . . ?
C8 C9 Br5 118.6(12) . . ?
C56 C57 C58 124(3) . . ?
C56 C57 Br37 117(3) . . ?
C58 C57 Br37 118(2) . . ?
C32 O12 Bi6 115.8(17) . . ?
C19 C24 C23 124(3) . . ?
C19 C24 Br16 121(3) . . ?
C23 C24 Br16 115(2) . . ?
C37 C38 C39 120.0 . . ?
C37 C38 O14 113.5(16) . . ?
C39 C38 O14 126.4(16) . . ?
O13 C37 C38 117.5(18) . . ?
O13 C37 C42 122.5(18) . . ?
C38 C37 C42 120.0 . . ?
C41 C42 C37 120.0 . . ?
C41 C42 Br28 121.0(11) . . ?
C37 C42 Br28 119.0(11) . . ?
C40 C41 C42 120.0 . . ?
C40 C41 Br27 117.5(11) . . ?
C42 C41 Br27 122.5(11) . . ?
C41 C40 C39 120.0 . . ?
C41 C40 Br26 120.6(11) . . ?
C39 C40 Br26 119.4(11) . . ?
C40 C39 C38 120.0 . . ?
C40 C39 Br25 123.5(11) . . ?
C38 C39 Br25 116.3(11) . . ?
O9 C25 C26 122(3) . . ?
O9 C25 C30 120(3) . . ?
C26 C25 C30 118(3) . . ?
C44 C43 O15 123(3) . . ?
C44 C43 C48 111(3) . . ?
O15 C43 C48 126(3) . . ?
C22 C21 C20 118(3) . . ?
C22 C21 Br13 126(3) . . ?
C20 C21 Br13 116(3) . . ?
C38 O14 Bi7 113.7(16) . . ?
C38 O14 Bi4 123.4(17) . . ?
Bi7 O14 Bi4 112.8(13) . . ?
C55 O19 Bi10 113(2) . . ?
C19 O7 Bi4 116(2) . . ?
C25 O9 Bi5 112(2) . . ?
C48 C47 C46 122(4) . . ?
C48 C47 Br31 114(3) . . ?
C46 C47 Br31 119(4) . . ?
C26 O10 Bi5 113(2) . . ?
C26 O10 Bi2 113(2) . . ?
Bi5 O10 Bi2 117.8(14) . . ?
O19 C55 C60 122(3) . . ?
O19 C55 C56 120(4) . . ?
C60 C55 C56 118(3) . . ?
O7 C19 C24 122(3) . . ?
O7 C19 C20 119(3) . . ?
C24 C19 C20 118(4) . . ?
C53 C54 C49 120(3) . . ?
C53 C54 Br36 123(2) . . ?
C49 C54 Br36 117(2) . . ?
C20 O8 Bi4 116.5(19) . . ?
C20 O8 Bi1 123.0(19) . . ?
Bi4 O8 Bi1 110.3(12) . . ?
C29 C30 C25 120(3) . . ?
C29 C30 Br20 123(2) . . ?
C25 C30 Br20 117(2) . . ?
O8 C20 C19 112(3) . . ?
O8 C20 C21 125(3) . . ?
C19 C20 C21 123(3) . . ?
C24 C23 C22 113(3) . . ?
C24 C23 Br15 128(2) . . ?
C22 C23 Br15 119(2) . . ?
C44 O16 Bi8 107(2) . . ?
C44 O16 Bi5 114(2) . . ?
Bi8 O16 Bi5 113.5(14) . . ?
C1 O1 Bi1 115.2(18) . . ?
O18 C50 C51 126(3) . . ?
O18 C50 C49 111(2) . . ?
C51 C50 C49 123(2) . . ?
C31 O11 Bi6 113.0(18) . . ?
C31 O11 Bi3 116.6(19) . . ?
Bi6 O11 Bi3 110.2(12) . . ?
C57 C56 C55 119(4) . . ?
C57 C56 O20 117(3) . . ?
C55 C56 O20 124(3) . . ?
C15 C14 C13 120.0 . . ?
C15 C14 O6 126(2) . . ?
C13 C14 O6 113(2) . . ?
C14 C15 C16 120.0 . . ?
C14 C15 Br9 118.5(15) . . ?
C16 C15 Br9 121.5(15) . . ?
C15 C16 C17 120.0 . . ?
C15 C16 Br10 119.8(15) . . ?
C17 C16 Br10 120.1(15) . . ?
C18 C17 C16 120.0 . . ?
C18 C17 Br11 119.9(16) . . ?
C16 C17 Br11 120.1(16) . . ?
C17 C18 C13 120.0 . . ?
C17 C18 Br12 122.2(15) . . ?
C13 C18 Br12 117.7(15) . . ?
C18 C13 C14 120.0 . . ?
C18 C13 O5 115(2) . . ?
C14 C13 O5 125(2) . . ?
O10 C26 C25 115(3) . . ?
O10 C26 C27 124(3) . . ?
C25 C26 C27 121(3) . . ?
C21 C22 C23 123(3) . . ?
C21 C22 Br14 119(3) . . ?
C23 C22 Br14 117(2) . . ?
C47 C48 C43 122(3) . . ?
C47 C48 Br32 127(3) . . ?
C43 C48 Br32 110(3) . . ?
C50 O18 Bi9 119.8(19) . . ?
C44 C45 C46 121(3) . . ?
C44 C45 Br29 121(3) . . ?
C46 C45 Br29 118(3) . . ?
C56 O20 Bi10 104(2) . . ?
C56 O20 Bi7 119(3) . . ?
Bi10 O20 Bi7 111.3(16) . . ?
C59 C60 C55 127(4) . . ?
C59 C60 Br40 118(3) . . ?
C55 C60 Br40 115(3) . . ?
C49 O17 Bi9 115.6(18) . . ?
C49 O17 Bi6 113.5(18) . . ?
Bi9 O17 Bi6 112.5(11) . . ?
C54 C53 C52 121(3) . . ?
C54 C53 Br35 120(2) . . ?
C52 C53 Br35 118(2) . . ?
C36 C31 C32 120.0 . . ?
C36 C31 O11 120.7(18) . . ?
C32 C31 O11 119.3(18) . . ?
C35 C36 C31 120.0 . . ?
C35 C36 Br24 124.1(12) . . ?
C31 C36 Br24 115.9(12) . . ?
C36 C35 C34 120.0 . . ?
C36 C35 Br23 119.0(13) . . ?
C34 C35 Br23 120.9(13) . . ?
C33 C34 C35 120.0 . . ?
C33 C34 Br22 119.6(12) . . ?
C35 C34 Br22 119.8(12) . . ?
C34 C33 C32 120.0 . . ?
C34 C33 Br21 121.6(12) . . ?
C32 C33 Br21 118.3(12) . . ?
C33 C32 C31 120.0 . . ?
C33 C32 O12 122.7(18) . . ?
C31 C32 O12 116.9(18) . . ?
C28 C27 C26 119(3) . . ?
C28 C27 Br17 125(3) . . ?
C26 C27 Br17 116(2) . . ?
C8 O4 Bi2 109.3(18) . . ?
C8 O4 Bi9 110.8(18) . 2_655 ?
Bi2 O4 Bi9 109.1(13) . 2_655 ?
C27 C28 C29 117(3) . . ?
C27 C28 Br18 119(3) . . ?
C29 C28 Br18 124(2) . . ?
C45 C44 C43 126(3) . . ?
C45 C44 O16 118(3) . . ?
C43 C44 O16 117(3) . . ?
C13 O5 Bi3 108(2) . . ?
C50 C51 C52 120(3) . . ?
C50 C51 Br33 120(2) . . ?
C52 C51 Br33 120(2) . . ?
C6 C1 C2 120.0 . . ?
C6 C1 O1 113(2) . . ?
C2 C1 O1 126(2) . . ?
O2 C6 C1 117(2) . . ?
O2 C6 C5 123(2) . . ?
C1 C6 C5 120.0 . . ?
C4 C5 C6 120.0 . . ?
C4 C5 Br4 119.5(15) . . ?
C6 C5 Br4 120.5(15) . . ?
C5 C4 C3 120.0 . . ?
C5 C4 Br3 121.7(15) . . ?
C3 C4 Br3 117.6(15) . . ?
C2 C3 C4 120.0 . . ?
C2 C3 Br2 116.5(15) . . ?
C4 C3 Br2 123.4(15) . . ?
C3 C2 C1 120.0 . . ?
C3 C2 Br1 123.4(15) . . ?
C1 C2 Br1 116.6(15) . . ?
C43 O15 Bi8 110(3) . . ?
Bi7 O24 Bi8 110.6(14) . . ?
Bi7 O24 Bi6 114.3(16) . . ?
Bi8 O24 Bi6 123.0(14) . . ?
C30 C29 C28 123(3) . . ?
C30 C29 Br19 119(3) . . ?
C28 C29 Br19 115(3) . . ?
C60 C59 C58 116(4) . . ?
C60 C59 Br39 127(3) . . ?
C58 C59 Br39 117(3) . . ?
C53 C52 C51 116(3) . . ?
C53 C52 Br34 121(2) . . ?
C51 C52 Br34 122(3) . . ?
Bi5 O23 Bi6 111.7(15) . . ?
Bi5 O23 Bi4 111.0(15) . . ?
Bi6 O23 Bi4 114.7(15) . . ?
Bi5 O23 Bi3 117.3(15) . . ?
Bi6 O23 Bi3 107.1(14) . . ?
Bi4 O23 Bi3 94.1(12) . . ?

_refine_diff_density_max         0.460
_refine_diff_density_min         -0.476
_refine_diff_density_rms         0.087



# start Validation Reply Form
_vrf_ATOM007_Bibrocathol-1-Monoclinic 
;
PROBLEM: _atom_site_aniso_label is missing
RESPONSE: The data quality of did not permit refinement of anisotropic
displacement parameters of such a complex structure.
;
_vrf_RINTA01_Bibrocathol-1-Monoclinic 
;
PROBLEM: The value of Rint is greater than 0.25
RESPONSE: Higher than expected R-values are commonly encountered for 3D ED
data, likely originating in dynamic diffraction effects (multiple scattering).
;
_vrf_PLAT020_Bibrocathol-1-Monoclinic 
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.278 Report
RESPONSE: Higher than expected R-values are commonly encountered for 3D ED
data, likely originating in dynamic diffraction effects (multiple scattering).
;
_vrf_PLAT082_Bibrocathol-1-Monoclinic 
;
PROBLEM: High R1 Value ..................................       0.23 Report
RESPONSE: Higher than expected R-values are commonly encountered for 3D ED
data, likely originating in dynamic diffraction effects (multiple scattering).
;
_vrf_PLAT084_Bibrocathol-1-Monoclinic 
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.56 Report
RESPONSE: Higher than expected R-values are commonly encountered for 3D ED
data, likely originating in dynamic diffraction effects (multiple scattering).
;
_vrf_PLAT342_Bibrocathol-1-Monoclinic 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.03917 Ang.
RESPONSE: The relatively low precision in unit cell parameters contributes to
the C-C bond precision.
;
_vrf_PLAT149_Bibrocathol-1-Monoclinic 
;
PROBLEM: s.u. on the   beta    Angle is Too Large .......       0.20 Degree
RESPONSE: We have added an empirically determined s.u. on the unit cell angle
and axes, as determined from large amounts of data from the same measurement
setup. This s.u. is large, as to not underestimate the potential uncertainty.
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Bibrocathol-2-Tetragonal
_database_code_depnum_ccdc_archive 'CCDC 2190212'
loop_
_audit_author_name
_audit_author_address
'Erik Svensson Grape'
;Stockholm University
Sweden
;
_audit_update_record             
;
2022-08-17 deposited with the CCDC.	2022-08-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 Bi Br8 O5'
_chemical_formula_weight         1072.34

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Bi Bi 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   25.16(13)
_cell_length_b                   25.16(13)
_cell_length_c                   13.98(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8850(99)
_cell_formula_units_Z            16
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    83501
_cell_measurement_theta_min      0.057
_cell_measurement_theta_max      0.892

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.219
_exptl_crystal_F_000             1753
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    0.000
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.0251
_diffrn_radiation_type           electron
_diffrn_source                   ?
_diffrn_measurement_device_type  'JEOL JEM-2100 LaB6'
_diffrn_measurement_method       'continuous rotation'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            83501
_diffrn_reflns_av_unetI/netI     0.2091
_diffrn_reflns_av_R_equivalents  0.5154
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         0.057
_diffrn_reflns_theta_max         0.892
_diffrn_reflns_theta_full        0.863
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.942
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             4171
_reflns_number_gt                3124
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       
;
Stef Smeets, Bin Wang, Magdalena O. Cichocka, Jonas Angstrom, Wei Wan.
(2018, April 11). Instamatic (Version 0.6). Zenodo.
http://doi.org/10.5281/zenodo.1217026
;
_computing_cell_refinement       
;
Kabsch, W. (2010). XDS. Acta Crystallographica Section D:
Biological Crystallography, 66(2), 125-132.
;
_computing_data_reduction        
;
Kabsch, W. (2010). XDS. Acta Crystallographica Section D:
Biological Crystallography, 66(2), 125-132.
;
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0584P)²+2.0578P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4171
_refine_ls_number_parameters     237
_refine_ls_number_restraints     76
_refine_ls_R_factor_all          0.2537
_refine_ls_R_factor_gt           0.2112
_refine_ls_wR_factor_ref         0.4293
_refine_ls_wR_factor_gt          0.4127
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_restrained_S_all      1.120
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001

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
Bi1 Bi 0.30210(14) 0.50872(14) 0.2878(2) 0.068(2) Uani 1 1 d . . . . .
Br1 Br 0.3602(4) 0.5149(3) -0.0840(4) 0.089(3) Uani 1 1 d . . . . .
Br2 Br 0.4201(3) 0.6291(3) -0.1366(4) 0.074(3) Uani 1 1 d . . . . .
Br3 Br 0.4285(3) 0.7242(3) 0.0307(5) 0.078(3) Uani 1 1 d . . . . .
Br4 Br 0.3858(3) 0.6962(3) 0.2530(5) 0.075(3) Uani 1 1 d . . . . .
Br5 Br 0.4674(3) 0.3840(3) 0.3053(5) 0.085(3) Uani 1 1 d D . . . .
Br6 Br 0.5260(3) 0.3824(4) 0.5199(6) 0.101(3) Uani 1 1 d . . . . .
Br7 Br 0.4784(4) 0.4631(3) 0.6933(5) 0.088(3) Uani 1 1 d . . . . .
Br8 Br 0.3682(3) 0.5321(3) 0.6518(4) 0.087(3) Uani 1 1 d . . . . .
O1 O 0.3494(11) 0.5772(9) 0.2635(11) 0.096(8) Uani 1 1 d . . . . .
O2 O 0.3331(7) 0.5063(7) 0.1297(11) 0.063(4) Uani 1 1 d . . . . .
O3 O 0.3318(8) 0.5231(7) 0.4414(9) 0.065(5) Uani 1 1 d . . . . .
O4 O 0.3754(8) 0.4654(8) 0.3064(11) 0.074(5) Uani 1 1 d D . . . .
O5 O 0.3750(8) 0.4123(10) 0.1614(10) 0.098(8) Uani 1 1 d D . . . .
C1 C 0.3650(7) 0.5916(7) 0.1781(13) 0.056(5) Uani 1 1 d . U . . .
C2 C 0.3552(9) 0.5541(9) 0.1039(14) 0.070(6) Uani 1 1 d . U . . .
C3 C 0.3761(10) 0.5671(10) 0.0091(14) 0.076(6) Uani 1 1 d . U . . .
C4 C 0.3974(8) 0.6166(9) -0.0139(12) 0.063(5) Uani 1 1 d . U . . .
C5 C 0.4016(10) 0.6609(11) 0.0592(15) 0.082(7) Uani 1 1 d . U . . .
C6 C 0.3840(8) 0.6442(8) 0.1570(15) 0.065(5) Uani 1 1 d . U . . .
C7 C 0.3741(9) 0.4940(8) 0.4591(12) 0.064(5) Uani 1 1 d . U . . .
C8 C 0.3984(8) 0.4594(9) 0.3867(11) 0.062(5) Uani 1 1 d . U . . .
C9 C 0.4418(8) 0.4277(10) 0.4097(14) 0.071(6) Uani 1 1 d . U . . .
C10 C 0.4695(8) 0.4243(9) 0.4948(17) 0.072(6) Uani 1 1 d . U . . .
C11 C 0.4478(8) 0.4603(9) 0.5675(16) 0.068(6) Uani 1 1 d . U . . .
C12 C 0.4015(10) 0.4899(8) 0.5522(14) 0.073(6) Uani 1 1 d . U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Bi1 O1 2.12(3) . ?
Bi1 O4 2.16(2) . ?
Bi1 O3 2.302(17) . ?
Bi1 O2 2.346(19) . ?
Br1 C3 1.89(2) . ?
Br2 C4 1.835(19) . ?
Br3 C5 1.78(3) . ?
Br4 C6 1.88(2) . ?
Br5 C9 1.94(2) . ?
Br6 C10 1.80(2) . ?
Br7 C11 1.92(2) . ?
Br8 C12 1.94(2) . ?
O1 C1 1.31(3) . ?
O2 C2 1.37(3) . ?
O3 C7 1.32(3) . ?
O4 C8 1.27(2) . ?
C1 C2 1.43(3) . ?
C1 C6 1.44(3) . ?
C2 C3 1.46(3) . ?
C3 C4 1.39(3) . ?
C4 C5 1.52(3) . ?
C5 C6 1.50(3) . ?
C7 C8 1.47(3) . ?
C7 C12 1.48(3) . ?
C8 C9 1.39(3) . ?
C9 C10 1.38(3) . ?
C10 C11 1.47(3) . ?
C11 C12 1.40(3) . ?

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
O1 Bi1 O4 87.2(8) . . ?
O1 Bi1 O3 80.8(7) . . ?
O4 Bi1 O3 71.9(6) . . ?
O1 Bi1 O2 71.5(6) . . ?
O4 Bi1 O2 79.4(6) . . ?
O3 Bi1 O2 140.8(7) . . ?
C1 O1 Bi1 122.7(15) . . ?
C2 O2 Bi1 111.1(12) . . ?
C7 O3 Bi1 110.5(12) . . ?
C8 O4 Bi1 123.7(13) . . ?
O1 C1 C2 115(2) . . ?
O1 C1 C6 122.9(18) . . ?
C2 C1 C6 121.2(18) . . ?
O2 C2 C1 117.4(18) . . ?
O2 C2 C3 125.5(18) . . ?
C1 C2 C3 117(2) . . ?
C4 C3 C2 123.3(18) . . ?
C4 C3 Br1 122.8(15) . . ?
C2 C3 Br1 113.0(17) . . ?
C3 C4 C5 121.9(17) . . ?
C3 C4 Br2 119.3(14) . . ?
C5 C4 Br2 118.8(16) . . ?
C6 C5 C4 113(2) . . ?
C6 C5 Br3 124.7(16) . . ?
C4 C5 Br3 122.3(16) . . ?
C1 C6 C5 123.0(18) . . ?
C1 C6 Br4 120.2(15) . . ?
C5 C6 Br4 116.8(16) . . ?
O3 C7 C8 122.5(17) . . ?
O3 C7 C12 125.6(16) . . ?
C8 C7 C12 111.9(18) . . ?
O4 C8 C9 129.0(18) . . ?
O4 C8 C7 110.4(18) . . ?
C9 C8 C7 120.5(17) . . ?
C10 C9 C8 129(2) . . ?
C10 C9 Br5 116.5(17) . . ?
C8 C9 Br5 114.4(14) . . ?
C9 C10 C11 111.8(19) . . ?
C9 C10 Br6 126.9(19) . . ?
C11 C10 Br6 121.3(16) . . ?
C12 C11 C10 122.2(19) . . ?
C12 C11 Br7 117.0(16) . . ?
C10 C11 Br7 120.5(14) . . ?
C11 C12 C7 124.1(19) . . ?
C11 C12 Br8 122.8(15) . . ?
C7 C12 Br8 113.1(16) . . ?

_refine_diff_density_max         0.042
_refine_diff_density_min         -0.053
_refine_diff_density_rms         0.010



# start Validation Reply Form
_vrf_RINTA01_Bibrocathol-2-Tetragonal 
;
PROBLEM: The value of Rint is greater than 0.25
RESPONSE: Higher than expected R-values are commonly encountered for 3D ED
data, likely originating in dynamic diffraction effects (multiple scattering).
;
_vrf_PLAT020_Bibrocathol-2-Tetragonal 
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.515 Report
RESPONSE: Higher than expected R-values are commonly encountered for 3D ED
data, likely originating in dynamic diffraction effects (multiple scattering).
;
_vrf_PLAT082_Bibrocathol-2-Tetragonal 
;
PROBLEM: High R1 Value ..................................       0.21 Report
RESPONSE: Higher than expected R-values are commonly encountered for 3D ED
data, likely originating in dynamic diffraction effects (multiple scattering).
;
_vrf_PLAT084_Bibrocathol-2-Tetragonal 
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.43 Report
RESPONSE: Higher than expected R-values are commonly encountered for 3D ED
data, likely originating in dynamic diffraction effects (multiple scattering).
;
_vrf_PLAT306_Bibrocathol-2-Tetragonal 
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......         O5 Check
RESPONSE: Hydrogen atoms could not be found in the difference Fourier map,
and as such they were not inferred geometrically.
;
_vrf_PLAT342_Bibrocathol-2-Tetragonal 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............       0.03 Ang.
RESPONSE: The inaccuracy of the determined unit cell parameters also affects
the C-C bond precision.
;
# end Validation Reply Form
