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_7226590
_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         '0.5(I20 Pb6), 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           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-03-09
_audit_creation_method
;
Olex2 1.2
(compiled Feb 16 2016 13:09:46 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-07-25 deposited with the CCDC.
2016-09-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.175(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.0812(11)
_cell_length_b                   22.600(2)
_cell_length_c                   8.8122(8)
_cell_measurement_reflns_used    7640
_cell_measurement_temperature    180.15
_cell_measurement_theta_max      26.03
_cell_measurement_theta_min      1.72
_cell_volume                     2351.9(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    'ShelXT (Sheldrick, 2015)'
_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 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1481
_diffrn_reflns_av_unetI/netI     0.1347
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            10560
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        25.742
_diffrn_reflns_theta_max         25.742
_diffrn_reflns_theta_min         1.724
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-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    20.691
_exptl_absorpt_correction_T_max  0.4076
_exptl_absorpt_correction_T_min  0.0364
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.568
_exptl_crystal_description       plate
_exptl_crystal_F_000             2168
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.137
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.658
_refine_diff_density_min         -3.340
_refine_diff_density_rms         0.441
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         4407
_refine_ls_number_restraints     108
_refine_ls_restrained_S_all      0.968
_refine_ls_R_factor_all          0.1360
_refine_ls_R_factor_gt           0.0800
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1879
_refine_ls_wR_factor_ref         0.2140
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2269
_reflns_number_total             4407
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce01684g2.cif
_cod_data_source_block           vp-50
_cod_depositor_comments
'Adding full bibliography for 7226587--7226601.cif.'
_cod_database_code               7226590
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 C6-Br2 \\sim C2AB-Br0A \\sim C1-Br1
 with sigma of 0.02
 C7-Br2 \\sim Br2-C8 \\sim C3A-Br0A \\sim Br0A-C10A \\sim C2-Br1 \\sim Br1-C3
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C9) = Uanis(C5A) = Uanis(C7) = Uanis(C3A) = Uanis(C6) = Uanis(C2AB) =
Uanis(C8) = Uanis(C10A) = Uanis(C10) = Uanis(C7A)
Uanis(N2) = Uanis(N4A)
Uanis(N2) = Uanis(N4A)
4. Rigid body (RIGU) restrains
 N4A, Br2, C6, C8, C7, C10, C9, N2, C7A, Br0A, C2AB, C10A, C3A, C5A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(Br0A)=Sof(C2AB)=Sof(C10A)=Sof(H10A)=Sof(C7A)=Sof(H7A)=Sof(N4A)=Sof(H4A)=
 Sof(C5A)=Sof(H5A)=Sof(C3A)=Sof(H3A)=1-FVAR(1)
 Sof(Br2)=Sof(C6)=Sof(C8)=Sof(H8)=Sof(C10)=Sof(H10)=Sof(N2)=Sof(H2A)=Sof(C9)=
 Sof(H9)=Sof(C7)=Sof(H7)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C2(H2), C4(H4), N1(H1), C5(H5), C8(H8), C10(H10), N2(H2A), C9(H9),
 C7(H7), C10A(H10A), C7A(H7A), N4A(H4A), C5A(H5A), C3A(H3A)
6.b Fitted hexagon refined as free rotating group:
 C3(C1,C2,C4,N1,C5), C6(C8,C10,N2,C9,C7), C2AB(C10A,C7A,N4A,C5A,C3A)
;
_olex2_submission_special_instructions 'No special instructions were received'