Structural diversity in substituted-pyridinium iodo- and bromoplumbates: a matter of halide and temperature
Gómez, Verónica; Fuhr, Olaf; Ruben, Mario; CrystEngComm 18 (2016) 8207–; doi:10.1039/C6CE01684G

data_7226588
_publ_section_title
;
 Structural diversity in substituted-pyridinium iodo- and bromoplumbates:
 a matter of halide and temperature
;
_journal_issue                   42
_journal_name_full               CrystEngComm
_journal_page_first              8207
_journal_paper_doi               10.1039/C6CE01684G
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'I10 Pb3, 4(C5 H5 Br N)'
_chemical_formula_sum            'C20 H20 Br4 I10 N4 Pb3'
_chemical_formula_weight         2526.61
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-11-26
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-07-25 deposited with the CCDC.
2016-09-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.617(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   23.010(2)
_cell_length_b                   9.6665(7)
_cell_length_c                   11.1481(12)
_cell_measurement_reflns_used    14896
_cell_measurement_temperature    180.15
_cell_measurement_theta_max      26.09
_cell_measurement_theta_min      1.92
_cell_volume                     2363.3(4)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      180.15
_diffrn_detector                 'image plate ( 34 cm diameter )'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.950
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_unetI/netI     0.0241
_diffrn_reflns_Laue_measured_fraction_full 0.950
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7187
_diffrn_reflns_point_group_measured_fraction_full 0.950
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.617
_diffrn_reflns_theta_min         2.229
_diffrn_source                   'sealed X-ray tube, 12 x 0.4 mm fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.000
_diffrn_source_target            Mo
_diffrn_source_type              'sealed X-ray tube'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    20.591
_exptl_absorpt_correction_T_max  0.1806
_exptl_absorpt_correction_T_min  0.0308
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.551
_exptl_crystal_description       needle
_exptl_crystal_F_000             2168
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.893
_refine_diff_density_min         -1.146
_refine_diff_density_rms         0.169
_refine_ls_extinction_coef       0.00224(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     111
_refine_ls_number_reflns         2341
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0245
_refine_ls_R_factor_gt           0.0232
_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^)+(0.0316P)^2^+4.2525P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0559
_refine_ls_wR_factor_ref         0.0564
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2230
_reflns_number_total             2341
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce01684g2.cif
_cod_data_source_block           vp-68
_cod_depositor_comments
'Adding full bibliography for 7226587--7226601.cif.'
_cod_database_code               7226588
_shelxl_version_number           2014/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Shared sites
{N2, C7}
{N1, C3}
3. Uiso/Uaniso restraints and constraints
Uanis(N1) = Uanis(C3)
Uanis(N2) = Uanis(C7)
4. Others
 Fixed Sof: N1(0.5) H1(0.5) C3(0.5) H3(0.5) H2A(0.5) H2B(0.5) H4A(0.25)
 H4B(0.25) N2(0.5) H2(0.5) H6A(0.5) H6B(0.5) H8A(0.25) H8B(0.25) C7(0.5) H7(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C3(H3), C2(H2A), C2(H2B), C4(H4A), C4(H4B), N2(H2), C6(H6A), C6(H6B),
 C8(H8A), C8(H8B), C7(H7)
;
_shelx_res_checksum              18469
_olex2_submission_special_instructions 'No special instructions were received'