Unusual isostructural Br/I substitution effect on the crystal structure and optical properties of hybrid halobismuthates
Kotov, Vitalii Yu.; Lunkov, Ivan S.; Buikin, Petr A.; Kottsov, Sergey Yu.; Korlyukov, Alexander A.; Rudenko, Alexander Yu.; New Journal of Chemistry 47 (2023) 2666–2672; doi:10.1039/D2NJ05184B

data_7062219
_publ_section_title
;
 Unusual isostructural Br/I substitution effect on the crystal structure
 and optical properties of hybrid halobismuthates
;
_journal_issue                   5
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              2666
_journal_page_last               2672
_journal_paper_doi               10.1039/D2NJ05184B
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'Bi Br4.389 I0.611, C14 H18 N2'
_chemical_formula_sum            'C14 H18 Bi Br4.39 I0.61 N2'
_chemical_formula_weight         851.61
_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
_audit_creation_date             2022-12-21
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-12-21 deposited with the CCDC.	2023-01-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.349(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0767(8)
_cell_length_b                   11.5480(9)
_cell_length_c                   14.9324(10)
_cell_measurement_reflns_used    4808
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.922
_cell_measurement_theta_min      2.444
_cell_volume                     2080.7(3)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/6 (Sheldrick, 2015)'
_computing_structure_solution    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.00
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Quest'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0590
_diffrn_reflns_av_unetI/netI     0.0611
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14073
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.012
_diffrn_reflns_theta_min         2.127
_exptl_absorpt_coefficient_mu    17.805
_exptl_absorpt_correction_T_max  0.0955
_exptl_absorpt_correction_T_min  0.0575
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1011 before and 0.0577 after correction.
The Ratio of minimum to maximum transmission is 0.6021.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.719
_exptl_crystal_description       needle
_exptl_crystal_F_000             1540
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.002
_refine_diff_density_max         1.174
_refine_diff_density_min         -1.205
_refine_diff_density_rms         0.222
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         4091
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0387
_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/[\s^2^(Fo^2^)+(0.0068P)^2^+3.4272P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0573
_refine_ls_wR_factor_ref         0.0609
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3331
_reflns_number_total             4091
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj05184b2.cif
_cod_data_source_block           pic2_bibri_0025
_cod_depositor_comments
'Adding full bibliography for 7062219--7062222.cif.'
_cod_database_code               7062219
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.965
_shelx_estimated_absorpt_t_min   0.470
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 I2-Bi1
 2.95 with sigma of 0.02
 Bi1-I1
 2.85 with sigma of 0.02
 I3-Bi1
 2.9 with sigma of 0.02
 Br4-Bi1
 3.08 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Br4) = Uanis(I4)
Uanis(I1) = Uanis(Br1)
Uanis(I3) = Uanis(Br3)
Uanis(Br2) = Uanis(I2)
4. Others
 Fixed Sof: I1(0.10696) I2(0.04503) I3(0.05277) I4(0.40663) Br1(0.89304)
 Br2(0.95497) Br3(0.94723) Br4(0.59337)
5.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C9(H9), C10(H10), C12(H12), C13(H13)
5.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C14(H14A,H14B,H14C)
;
_shelx_res_checksum              44131
_olex2_submission_special_instructions 'No special instructions were received'