Synthetic strategy towards halometallates with imidazo[1,5-a]pyridinium-based counterions
Vassilyeva, Olga Yu.; Buvaylo, Elena A.; Linnik, Rostyslav P.; Nesterov, Dmytro S.; Trachevsky, Vladimir V.; Skelton, Brian W.; CrystEngComm  (2020) –; doi:10.1039/D0CE00018C

data_7240910
_publ_section_title
;
 Synthetic strategy towards halometallates with
 imidazo[1,5-a]pyridinium-based counterions
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE00018C
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         'Cl3 Pb, C8 H9 N2'
_chemical_formula_sum            'C8 H9 Cl3 N2 Pb'
_chemical_formula_weight         446.71
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      43
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-12-21T06:13:32-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2019-12-16 deposited with the CCDC.	2020-07-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   43.5467(12)
_cell_length_b                   24.8590(7)
_cell_length_c                   4.32220(10)
_cell_measurement_reflns_used    7782
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.178
_cell_measurement_theta_min      1.903
_cell_volume                     4678.9(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Diamond (Brandenburg, K., (1999)'
_computing_publication_material  'WinGX Farrugia, L. J. (1999)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4738
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Gemini diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.013616
_diffrn_orient_matrix_UB_12      -0.0039519
_diffrn_orient_matrix_UB_13      -0.0871415
_diffrn_orient_matrix_UB_21      -0.0003442
_diffrn_orient_matrix_UB_22      0.0273546
_diffrn_orient_matrix_UB_23      -0.0465275
_diffrn_orient_matrix_UB_31      0.0089327
_diffrn_orient_matrix_UB_32      0.0070874
_diffrn_orient_matrix_UB_33      0.1310434
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0404
_diffrn_reflns_av_unetI/netI     0.1033
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       62
_diffrn_reflns_limit_h_min       -51
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            13122
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        31
_diffrn_reflns_theta_max         32.436
_diffrn_reflns_theta_min         1.871
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    15.07
_exptl_absorpt_correction_T_max  0.332
_exptl_absorpt_correction_T_min  0.073
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
         CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.537
_exptl_crystal_description       needle
_exptl_crystal_F_000             3264
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.085
_refine_diff_density_max         0.767
_refine_diff_density_min         -1.109
_refine_diff_density_rms         0.236
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.360(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.875
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     129
_refine_ls_number_reflns         3868
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.875
_refine_ls_R_factor_all          0.026
_refine_ls_R_factor_gt           0.0204
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w=1/[\s^2^(Fo^2^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0304
_refine_ls_wR_factor_ref         0.0318
_reflns_number_gt                3663
_reflns_number_total             3868
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce00018c2.cif
_cod_data_source_block           lv744f
_cod_database_code               7240910
_shelx_res_checksum              87609