#------------------------------------------------------------------------------
#$Date: 2019-12-24 02:06:54 +0200 (Tue, 24 Dec 2019) $
#$Revision: 245527 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/38/4133829.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_4133829
loop_
_publ_author_name
'García-Sánchez, Alba'
'Gomez-Mendoza, Miguel'
'Barawi, Mariam'
'Villar-Garcia, Ignacio Jose'
'Liras, Marta'
'Gándara, Felipe'
'de la Peña O'Shea, Víctor A'
_publ_section_title
;
 Fundamental Insights in Photoelectrocatalytic Hydrogen Production with a
 Hole-transport Bismuth Metal-organic Framework.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b10261
_journal_year                    2019
_chemical_formula_moiety         '2(C40 H8 Bi2 O16 S12)'
_chemical_formula_sum            'C80 H Bi4 O32 S24'
_chemical_formula_weight         3079.17
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-08-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   24.257(5)
_cell_length_b                   15.144(3)
_cell_length_c                   10.676(2)
_cell_measurement_reflns_used    9970
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      65.17
_cell_measurement_theta_min      4.52
_cell_volume                     3921.8(13)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0494
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            21678
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        65.333
_diffrn_reflns_theta_max         65.333
_diffrn_reflns_theta_min         4.525
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    12.071
_exptl_absorpt_correction_T_max  0.5835
_exptl_absorpt_correction_T_min  0.3005
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1413 before and 0.0800 after correction. The Ratio of minimum to maximum transmission is 0.5150. The λ/2 correction factor is Not present.'
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_F_000             1453
_refine_diff_density_max         4.825
_refine_diff_density_min         -2.289
_refine_diff_density_rms         0.274
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.181
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         3472
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.180
_refine_ls_R_factor_all          0.0802
_refine_ls_R_factor_gt           0.0761
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1178P)²+77.7462P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2404
_refine_ls_wR_factor_ref         0.2441
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3203
_reflns_number_total             3472
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja9b10261_si_002.cif
_cod_data_source_block           ag125_a_0m_a
_cod_original_cell_volume        3921.9(13)
_cod_database_code               4133829
_shelx_shelxl_version_number     2018/3
_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.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid bond restraints
 C00C, C00F, C00J, C00G
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
3.a Aromatic/amide H refined with riding coordinates:
 C00J(H00J), C00M(H00M), C00R(H00R)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, 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
Bi01 Bi 0.73202(3) 0.750000 0.62461(6) 0.0369(3) Uani 1 2 d S T P
S002 S 0.71600(18) 0.3807(2) 0.7510(3) 0.0489(9) Uani 1 1 d . . .
S003 S 0.7879(3) 0.250000 0.4465(4) 0.0491(12) Uani 1 2 d S T P
S004 S 0.4059(3) 0.750000 0.1516(6) 0.0730(18) Uani 1 2 d S T P
S005 S 0.5316(3) 0.750000 0.3776(6) 0.088(3) Uani 1 2 d S T P
S006 S 0.5629(3) 0.750000 -0.0072(7) 0.115(4) Uani 1 2 d S T P
O007 O 0.3029(6) 0.750000 0.0132(13) 0.047(3) Uani 1 2 d S T P
O008 O 0.6920(6) 0.750000 0.4384(13) 0.056(4) Uani 1 2 d S T P
O009 O 0.7457(7) 0.6014(6) 0.5760(11) 0.077(4) Uani 1 1 d . . .
O00A O 0.7038(6) 0.5819(6) 0.7567(10) 0.069(3) Uani 1 1 d . . .
C00B C 0.7288(5) 0.5555(10) 0.6643(13) 0.039(3) Uiso 1 1 d . . .
C00C C 0.7398(6) 0.2976(8) 0.6544(12) 0.039(3) Uani 1 1 d . U .
O00D O 0.3360(7) 0.750000 -0.177(2) 0.096(7) Uani 1 2 d S T P
O00E O 0.6210(8) 0.750000 0.5722(18) 0.110(9) Uani 1 2 d S T P
C00F C 0.7635(6) 0.3314(8) 0.5475(13) 0.040(3) Uani 1 1 d . U .
C00G C 0.7390(7) 0.4590(9) 0.6445(12) 0.047(3) Uani 1 1 d . U .
C00H C 0.3429(9) 0.750000 -0.061(2) 0.062(6) Uani 1 2 d S T P
C00I C 0.6387(9) 0.750000 0.463(2) 0.058(6) Uani 1 2 d S T P
C00J C 0.7634(6) 0.4206(8) 0.5424(13) 0.042(3) Uani 1 1 d . U .
H00J H 0.778293 0.452640 0.476318 0.051 Uiso 1 1 calc R . .
C00K C 0.5217(10) 0.750000 0.218(2) 0.071(7) Uani 1 2 d S T P
C00L C 0.6033(10) 0.750000 0.356(2) 0.068(7) Uani 1 2 d S T P
C00M C 0.6172(11) 0.750000 0.234(2) 0.076(8) Uani 1 2 d S T P
H00M H 0.653282 0.750000 0.204284 0.091 Uiso 1 2 calc RS T P
C00N C 0.4781(10) 0.750000 0.136(2) 0.070(7) Uani 1 2 d S T P
C00O C 0.3985(10) 0.750000 -0.008(2) 0.068(7) Uani 1 2 d S T P
C00P C 0.5700(11) 0.750000 0.157(3) 0.082(8) Uani 1 2 d S T P
C00Q C 0.4905(10) 0.750000 0.013(3) 0.077(8) Uani 1 2 d S T P
C00R C 0.4467(11) 0.750000 -0.070(3) 0.092(10) Uani 1 2 d S T P
H00R H 0.450186 0.750000 -0.157203 0.111 Uiso 1 2 calc RS T P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Bi Bi -4.0111 8.9310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0181 0.0091 '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'
S S 0.3331 0.5567 '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'
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
O007 Bi01 O009 75.4(3) 6_656 7_575
O007 Bi01 O009 75.4(3) 6_656 .
O007 Bi01 O00D 52.9(6) 6_656 6_656
O007 Bi01 O00E 127.7(5) 6_656 .
O007 Bi01 C00H 26.4(6) 6_656 6_656
O007 Bi01 C00I 102.1(6) 6_656 .
O008 Bi01 O007 75.5(5) . 6_656
O008 Bi01 O009 82.1(4) . 7_575
O008 Bi01 O009 82.1(4) . .
O008 Bi01 O00D 128.4(6) . 6_656
O008 Bi01 O00E 52.2(6) . .
O008 Bi01 C00H 101.9(7) . 6_656
O008 Bi01 C00I 26.6(6) . .
O009 Bi01 O009 149.4(5) 7_575 .
O009 Bi01 O00D 84.8(4) 7_575 6_656
O009 Bi01 O00D 84.7(4) . 6_656
O009 Bi01 O00E 95.4(4) 7_575 .
O009 Bi01 O00E 95.4(4) . .
O009 Bi01 C00H 78.9(4) . 6_656
O009 Bi01 C00H 78.9(4) 7_575 6_656
O009 Bi01 C00I 88.8(4) 7_575 .
O009 Bi01 C00I 88.8(4) . .
O00D Bi01 O00E 179.3(6) 6_656 .
O00D Bi01 C00H 26.5(7) 6_656 6_656
O00D Bi01 C00I 155.1(7) 6_656 .
O00E Bi01 C00H 154.1(7) . 6_656
O00E Bi01 C00I 25.6(6) . .
C00H Bi01 C00I 128.6(7) 6_656 .
C00C S002 C00G 90.0(6) . .
C00F S003 C00F 90.2(9) . 7_565
C00O S004 C00N 90.5(12) . .
C00K S005 C00L 90.4(11) . .
C00P S006 C00Q 88.7(13) . .
C00H O007 Bi01 100.1(13) . 6_556
C00I O008 Bi01 104.5(12) . .
C00B O009 Bi01 108.9(9) . .
O009 C00B C00G 112.6(12) . .
O00A C00B O009 126.3(14) . .
O00A C00B C00G 121.0(13) . .
C00C C00C S002 136.8(4) 7_565 .
C00F C00C S002 111.3(9) . .
C00F C00C C00C 111.9(7) . 7_565
C00H O00D Bi01 85.4(15) . 6_556
C00I O00E Bi01 81.5(13) . .
C00C C00F S003 113.0(9) . .
C00J C00F S003 133.2(11) . .
C00J C00F C00C 113.8(12) . .
C00B C00G S002 121.4(10) . .
C00J C00G S002 111.7(10) . .
C00J C00G C00B 126.8(13) . .
O007 C00H Bi01 53.5(10) . 6_556
O007 C00H C00O 118(2) . .
O00D C00H Bi01 68.1(12) . 6_556
O00D C00H O007 122(2) . .
O00D C00H C00O 121(2) . .
C00O C00H Bi01 171.3(18) . 6_556
O008 C00I Bi01 48.8(9) . .
O008 C00I C00L 115(2) . .
O00E C00I Bi01 72.9(13) . .
O00E C00I O008 122(2) . .
O00E C00I C00L 123(2) . .
C00L C00I Bi01 164.2(17) . .
C00F C00J C00G 113.2(13) . .
C00N C00K S005 138(2) . .
C00P C00K S005 111.0(19) . .
C00P C00K C00N 111(2) . .
C00I C00L S005 119.3(18) . .
C00M C00L S005 112.1(19) . .
C00M C00L C00I 129(2) . .
C00L C00M C00P 111(2) . .
C00K C00N S004 135(2) . .
C00Q C00N S004 108.4(19) . .
C00Q C00N C00K 117(2) . .
C00H C00O S004 118.8(18) . .
C00R C00O S004 114(2) . .
C00R C00O C00H 128(2) . .
C00K C00P S006 113(2) . .
C00K C00P C00M 115(3) . .
C00M C00P S006 131(2) . .
C00N C00Q S006 109.8(19) . .
C00N C00Q C00R 117(2) . .
C00R C00Q S006 133(2) . .
C00O C00R C00Q 110(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Bi01 O007 2.263(14) 6_656
Bi01 O008 2.213(14) .
Bi01 O009 2.333(9) 7_575
Bi01 O009 2.333(9) .
Bi01 O00D 2.582(18) 6_656
Bi01 O00E 2.751(18) .
Bi01 C00H 2.77(2) 6_656
Bi01 C00I 2.85(2) .
S002 C00C 1.727(13) .
S002 C00G 1.736(14) .
S003 C00F 1.741(12) 7_565
S003 C00F 1.741(12) .
S004 C00N 1.76(2) .
S004 C00O 1.71(3) .
S005 C00K 1.72(3) .
S005 C00L 1.76(3) .
S006 C00P 1.76(3) .
S006 C00Q 1.77(3) .
O007 C00H 1.25(3) .
O008 C00I 1.32(3) .
O009 C00B 1.241(18) .
O00A C00B 1.225(17) .
C00B C00G 1.50(2) .
C00C C00C 1.44(2) 7_565
C00C C00F 1.378(19) .
O00D C00H 1.24(3) .
O00E C00I 1.24(3) .
C00F C00J 1.351(17) .
C00G C00J 1.369(19) .
C00H C00O 1.46(3) .
C00I C00L 1.43(3) .
C00K C00N 1.38(3) .
C00K C00P 1.34(4) .
C00L C00M 1.34(3) .
C00M C00P 1.41(4) .
C00N C00Q 1.35(4) .
C00O C00R 1.35(4) .
C00Q C00R 1.38(4) .
