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_7704084
_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         'Bi2 I9, 3(C H6 N)'
_chemical_formula_sum            'C3 H18 Bi2 I9 N3'
_chemical_formula_weight         1656.26
_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   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-12-19
_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                 91.647(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.4972(3)
_cell_length_b                   14.6869(5)
_cell_length_c                   21.5538(12)
_cell_measurement_reflns_used    3403
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.7560
_cell_measurement_theta_min      2.4330
_cell_volume                     2688.7(2)
_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(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.734
_diffrn_measured_fraction_theta_max 0.734
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w      0.00 360.00   0.25    2.00    --    0.00   0.00   0.00 1440
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dectris-CrysAlisPro-abstract goniometer imported dectris images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0476675000
_diffrn_orient_matrix_UB_12      0.0370785000
_diffrn_orient_matrix_UB_13      -0.0025302000
_diffrn_orient_matrix_UB_21      -0.0034084000
_diffrn_orient_matrix_UB_22      0.0022380000
_diffrn_orient_matrix_UB_23      0.0314656000
_diffrn_orient_matrix_UB_31      0.0642902000
_diffrn_orient_matrix_UB_32      0.0276835000
_diffrn_orient_matrix_UB_33      0.0009234000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6804
_diffrn_reflns_av_unetI/netI     0.0216
_diffrn_reflns_Laue_measured_fraction_full 0.734
_diffrn_reflns_Laue_measured_fraction_max 0.734
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            3917
_diffrn_reflns_point_group_measured_fraction_full 0.734
_diffrn_reflns_point_group_measured_fraction_max 0.734
_diffrn_reflns_theta_full        23.891
_diffrn_reflns_theta_max         23.891
_diffrn_reflns_theta_min         1.810
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    20.942
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44563
_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    4.092
_exptl_crystal_description       plate
_exptl_crystal_F_000             2800
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.025
_refine_diff_density_max         3.658
_refine_diff_density_min         -3.373
_refine_diff_density_rms         0.901
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.211
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         3917
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.206
_refine_ls_R_factor_all          0.0989
_refine_ls_R_factor_gt           0.0920
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2803
_refine_ls_wR_factor_ref         0.2867
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3144
_reflns_number_total             3917
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 60.0237\% 
 around [-0.00 0.00 -1.00] (reciprocal) or [-0.07 0.00 -1.00] (direct)
Component 3 rotated by -119.9933\% 
 around [0.00 -0.00 1.00] (reciprocal) or [0.08 0.00 1.00] (direct)
Component 4 rotated by 179.9846\% 
 around [1.00 0.00 -0.07] (reciprocal) or [1.00 0.00 -0.00] (direct)
;
_cod_data_source_file            d0dt00015a2.cif
_cod_data_source_block           Compound_2L_100K
_cod_depositor_comments
'Adding full bibliography for 7704084--7704087.cif.'
_cod_database_code               7704084
_shelx_shelxl_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C3 H18 Bi2 I9 N3'
_oxdiff_twin_items               4
_oxdiff_twin_integration_method  simultaneous
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.285(10)
 0.213(6) 0.188(6) 0.314(5)
2. Fixed Uiso
 At 1.2 times of:
  All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C3) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C2) \\sim
Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
4. Rigid body (RIGU) restrains
 C1, C2, C3, N1, N2, N3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), C1(H1D,H1E,H1F), N2(H2A,H2B,H2C), C2(H2D,H2E,H2F), N3(H3A,
 H3B,H3C), C3(H3D,H3E,H3F)
;