Zero-dimensional hybrid iodobismuthate derivatives: from structure study to photovoltaic application.
Zhang, Yi; Fadaei Tirani, Farzaneh; Pattison, Philip; Schenk-Joß, Kurt; Xiao, Zewen; Nazeeruddin, Mohammad Khaja; Gao, Peng; Dalton transactions (Cambridge, England : 2003) 49 (2020) 5815–5822; doi:10.1039/d0dt00015a

data_7704087
_publ_section_title
;
 Zero-dimensional hybrid iodobismuthate derivatives: from structure study
 to photovoltaic application.
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5815
_journal_page_last               5822
_journal_paper_doi               10.1039/d0dt00015a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'Bi I6, 6(C H6 N), 3(Cl)'
_chemical_formula_sum            'C6 H36 Bi Cl3 I6 N6'
_chemical_formula_weight         1269.14
_space_group_crystal_system      orthorhombic
_space_group_IT_number           67
_space_group_name_Hall           '-C 2a 2'
_space_group_name_H-M_alt        'C m m a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-12-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-04-01 deposited with the CCDC.	2020-04-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.94284(14)
_cell_length_b                   18.83413(12)
_cell_length_c                   9.13917(6)
_cell_measurement_reflns_used    10292
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      32.1830
_cell_measurement_theta_min      2.0800
_cell_volume                     3260.60(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.20a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.20a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.20a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(1)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \f      0.00 360.00   1.00    6.99   0.00   0.00   0.00    --   360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dectris-CrysAlisPro-abstract goniometer imported dectris images'
_diffrn_measurement_method       '\f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0291114000
_diffrn_orient_matrix_UB_12      -0.0187337000
_diffrn_orient_matrix_UB_13      0.0250642000
_diffrn_orient_matrix_UB_21      0.0043463000
_diffrn_orient_matrix_UB_22      -0.0244030000
_diffrn_orient_matrix_UB_23      -0.0560252000
_diffrn_orient_matrix_UB_31      0.0218116000
_diffrn_orient_matrix_UB_32      -0.0201852000
_diffrn_orient_matrix_UB_33      0.0446260000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6935
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_unetI/netI     0.0171
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            7614
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        24.589
_diffrn_reflns_theta_max         25.683
_diffrn_reflns_theta_min         2.098
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    10.668
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67163
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.20a (Rigaku Oxford Diffraction, 2018).
 Empirical absorption correction using spherical harmonics
 as implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.585
_exptl_crystal_description       plate
_exptl_crystal_F_000             2264
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.025
_refine_diff_density_max         1.044
_refine_diff_density_min         -1.387
_refine_diff_density_rms         0.170
_refine_ls_extinction_coef       0.000174(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     74
_refine_ls_number_reflns         1751
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0217
_refine_ls_R_factor_gt           0.0217
_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/[\s^2^(Fo^2^)+(0.0292P)^2^+30.8967P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0589
_refine_ls_wR_factor_ref         0.0589
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1751
_reflns_number_total             1751
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00015a2.cif
_cod_data_source_block           Compound_1_100K
_cod_depositor_comments
'Adding full bibliography for 7704084--7704087.cif.'
_cod_original_sg_symbol_Hall     '-C 2b 2'
_cod_original_sg_symbol_H-M      'C m m e'
_cod_database_code               7704087
_shelx_shelxl_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C6 H36 Bi Cl3 I6 N6'
_reflns_odcompleteness_completeness 98.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.69
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H) groups, All C(H,H,H) groups
2. Restrained distances
 N2-H2B = N2-H2A
 0.89 with sigma of 0.01
 C2-H2C = C2-H2D
 0.98 with sigma of 0.01
 H2A-H2B
 1.453 with sigma of 0.01
 H2C-H2D
 1.6 with sigma of 0.01
 N2-H2D
 2.031 with sigma of 0.01
 N2-H2C
 2.031 with sigma of 0.01
 C2-H2B
 1.981 with sigma of 0.01
 C2-H2A
 1.981 with sigma of 0.01
3.a Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), C1(H1D,H1E,H1F)
;
_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 1.500
_oxdiff_exptl_absorpt_empirical_full_min 0.647