Synthesis of a two-dimensional organic‒inorganic bismuth iodide metalate through in situ formation of iminium cations
Dehnhardt, Natalie; Luy, Jan-Niclas; Szabo, Marvin; Wende, Mirco; Tonner, Ralf; Heine, Johanna; Chemical Communications  (2019) –; doi:10.1039/C9CC06625J

data_7124429
_publ_section_title
;
 Synthesis of a two-dimensional organic--inorganic bismuth iodide metalate
 through in situ formation of iminium cations
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC06625J
_journal_year                    2019
_chemical_formula_moiety         'Bi2 I7, C5 H12 N'
_chemical_formula_sum            'C5 H12 Bi2 I7 N'
_chemical_formula_weight         1392.42
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-06-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-07-11 deposited with the CCDC.	2019-10-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.165(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.4647(8)
_cell_length_b                   7.5084(4)
_cell_length_c                   20.9965(11)
_cell_measurement_reflns_used    9996
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.30
_cell_measurement_theta_min      2.96
_cell_volume                     2166.7(2)
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 QUEST area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0623
_diffrn_reflns_av_unetI/netI     0.0180
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            83909
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.322
_diffrn_reflns_theta_min         2.713
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    26.177
_exptl_absorpt_correction_T_max  0.3311
_exptl_absorpt_correction_T_min  0.2865
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1022 before and 0.0607 after correction. The Ratio of minimum to maximum transmission is 0.8653. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    4.269
_exptl_crystal_description       block
_exptl_crystal_F_000             2344
_exptl_crystal_size_max          0.078
_exptl_crystal_size_mid          0.049
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.912
_refine_diff_density_min         -1.257
_refine_diff_density_rms         0.217
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         3936
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0222
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0130P)^2^+4.8387P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0352
_refine_ls_wR_factor_ref         0.0367
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3402
_reflns_number_total             3936
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc06625j2.cif
_cod_data_source_block           compound1
_cod_database_code               7124429
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.421
_shelx_estimated_absorpt_t_min   0.235
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H,H,H,H) groups
2. Shared sites
{C5, N5}
{C6, N6}
3. Uiso/Uaniso restraints and constraints
Uanis(C5) = Uanis(N5)
Uanis(C6) = Uanis(N6)
4. Others
 Sof(C5)=Sof(N6)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(H4AA)=Sof(H4AB)=Sof(H4AC)=
 Sof(H2AA)=Sof(H2AB)=Sof(H2AC)=Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=1-FVAR(1)
 Sof(N5)=Sof(C6)=Sof(H1BD)=Sof(H1BE)=Sof(H1BF)=Sof(H4BD)=Sof(H4BE)=Sof(H4BF)=
 Sof(H2BD)=Sof(H2BE)=Sof(H2BF)=Sof(H3BD)=Sof(H3BE)=Sof(H3BF)=FVAR(1)
5.a Idealised Me refined as rotating group:
 C1(H1BD,H1BE,H1BF), C1(H1AA,H1AB,H1AC), C4(H4AA,H4AB,H4AC), C4(H4BD,H4BE,
 H4BF), C2(H2BD,H2BE,H2BF), C2(H2AA,H2AB,H2AC), C3(H3AA,H3AB,H3AC), C3(H3BD,
 H3BE,H3BF)
;
_shelx_res_checksum              95611
_olex2_submission_special_instructions 'No special instructions were received'