A zero-dimensional lead-free bismuth-based metal halide: [C6H5(CH2)2CH(NH3)CH3]2BiCl5
Wei, Wen Juan; Gao, Hong Qiang; Tang, Yun Zhi; New Journal of Chemistry 46 (2022) 22999–23002; doi:10.1039/D2NJ04382C

data_7062087
_publ_section_title
;
 A zero-dimensional lead-free bismuth-based metal halide:
 [C6H5(CH2)2CH(NH3)CH3]2BiCl5
;
_journal_issue                   48
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              22999
_journal_page_last               23002
_journal_paper_doi               10.1039/D2NJ04382C
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'Bi Cl5, 2(C10 H16.014 N)'
_chemical_formula_sum            'C20 H32.01 Bi Cl5 N2'
_chemical_formula_weight         686.72
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-10-16
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-11-04 deposited with the CCDC.	2022-11-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.766(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.8036(12)
_cell_length_b                   12.8175(5)
_cell_length_c                   12.0035(6)
_cell_measurement_reflns_used    7935
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.5580
_cell_measurement_theta_min      3.8110
_cell_volume                     2797.5(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2137
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.891
_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    -75.00  30.00   1.00   21.49    --  -10.68 -19.00 150.00  105
  2  \w    -82.00  12.00   1.00   21.49    --  -10.68 -57.00 -60.00   94
  3  \w     -3.00  24.00   1.00   21.49    --  -10.68  38.00 120.00   27
  4  \w     20.00  60.00   1.00   21.49    --   11.22  19.00-150.00   40
  5  \w    -13.00  20.00   1.00   21.49    --   11.22 -99.00-180.00   33
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0168073000
_diffrn_orient_matrix_UB_12      -0.0387326000
_diffrn_orient_matrix_UB_13      0.0403461000
_diffrn_orient_matrix_UB_21      0.0352096000
_diffrn_orient_matrix_UB_22      0.0190042000
_diffrn_orient_matrix_UB_23      -0.0014163000
_diffrn_orient_matrix_UB_31      -0.0004816000
_diffrn_orient_matrix_UB_32      0.0346476000
_diffrn_orient_matrix_UB_33      0.0458512000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_unetI/netI     0.0434
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.891
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            22377
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.891
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.497
_diffrn_reflns_theta_min         3.361
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.789
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67003
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.122a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_description       block
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.142
_exptl_crystal_size_mid          0.021
_exptl_crystal_size_min          0.003
_refine_diff_density_max         1.222
_refine_diff_density_min         -0.598
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         6952
_refine_ls_number_restraints     198
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0338
_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^)+(0.0185P)^2^+1.6226P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0534
_refine_ls_wR_factor_ref         0.0616
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4976
_reflns_number_total             6952
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj04382c2.cif
_cod_data_source_block           qt-18-1-293k_auto
_cod_depositor_comments
'Adding full bibliography for 7062087--7062088.cif.'
_cod_database_code               7062087
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H,H,H)
  groups, All N(H,H,H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 H00A, H9A, H2A, H00B, H4AC, H00C, H5A, H3, H6AB, C8A, C3A, H2AA, C7, H1A,
 C12A, H4AA, H12A, H6AA, C11A, C2, H11A, H2C, C7A, C5A, H7A, C2A, C10A, C9A,
 H10A, C1A, C19A, C3, H19A, C4A, C12, H4AB, H12, C6A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 H00D, C1, H00E, H4BA, H00F, C9B, C8, C6, C19B, H4BC, H19B, C2B, C10B, C1B,
 H10B, C5B, C7B, H6B, H7B, H4BB, C11B, C6B, H11B, C3B, C12B, H2B, H12B, H9B, C0,
  H1B, H0, H1, C8B, H5B, H8BA, H6A, H8BB, C4B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(C8)=Sof(C19B)=Sof(H19B)=Sof(C10B)=Sof(H10B)=Sof(C7B)=Sof(H7B)=Sof(C11B)=
 Sof(H11B)=Sof(C12B)=Sof(H12B)=Sof(C8B)=Sof(H8BA)=Sof(H8BB)=1-FVAR(1)
 Sof(H00G)=Sof(H00H)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(C7)=Sof(C12A)=Sof(H12A)=
 Sof(C11A)=Sof(H11A)=Sof(C7A)=Sof(H7A)=Sof(C10A)=Sof(H10A)=Sof(C19A)=Sof(H19A)=
 FVAR(1)
 Sof(H00D)=Sof(H00E)=Sof(H00F)=Sof(H00I)=Sof(H00J)=Sof(C0)=Sof(H0)=1-FVAR(2)
 Sof(H00A)=Sof(H00B)=Sof(H00C)=Sof(C12)=Sof(H12)=FVAR(2)
 Sof(H00N)=Sof(C6B)=Sof(H6BA)=Sof(H6BB)=Sof(C3B)=Sof(C2B)=Sof(H2B)=Sof(C9B)=
 Sof(H9B)=Sof(C1B)=Sof(H1B)=Sof(C1)=Sof(H1)=Sof(C5B)=Sof(H5B)=Sof(C6)=Sof(H6A)=
 Sof(H6B)=1-FVAR(3)
 Sof(H009)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(C2)=Sof(H2A)=Sof(H2C)=Sof(C3A)=
 Sof(C5A)=Sof(H5A)=Sof(C2A)=Sof(H2AA)=Sof(C9A)=Sof(H9A)=Sof(C1A)=Sof(H1A)=
 Sof(C3)=Sof(H3)=FVAR(3)
 Sof(C4B)=Sof(H4BA)=Sof(H4BB)=Sof(H4BC)=1-FVAR(4)
 Sof(C4A)=Sof(H4AA)=Sof(H4AB)=Sof(H4AC)=FVAR(4)
4.a Ternary CH refined with riding coordinates:
 C009(H00N), C009(H009), C0(H0), C12(H12)
4.b Secondary CH2 refined with riding coordinates:
 C00A(H00I,H00J), C00A(H00G,H00H), C8B(H8BA,H8BB), C6B(H6BA,H6BB), C8A(H8AA,
 H8AB), C6(H6A,H6B), C6A(H6AA,H6AB), C2(H2A,H2C)
4.c Aromatic/amide H refined with riding coordinates:
 C19B(H19B), C10B(H10B), C7B(H7B), C11B(H11B), C12B(H12B), C12A(H12A),
 C11A(H11A), C7A(H7A), C10A(H10A), C19A(H19A), C2B(H2B), C9B(H9B), C1B(H1B),
 C1(H1), C5B(H5B), C5A(H5A), C2A(H2AA), C9A(H9A), C1A(H1A), C3(H3)
4.d Fitted hexagon refined as free rotating group:
 C8(C19B,C10B,C7B,C11B,C12B), C7(C12A,C11A,C7A,C10A,C19A), C3B(C2B,C9B,C1B,C1,
 C5B)
4.e Idealised Me refined as rotating group:
 N007(H00D,H00E,H00F), N007(H00A,H00B,H00C), N008(H00K,H00L,H00M), C00D(H00O,
 H00P,H00Q), C4B(H4BA,H4BB,H4BC), C4A(H4AA,H4AB,H4AC)
;
_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 1.598
_oxdiff_exptl_absorpt_empirical_full_min 0.774