Poly[bis(μ-5-iodoisophthalato)(methanol)dilead(II)] exhibiting a novel centrosymmetric rhombus-shaped I~4~ unit
Luo, Shao-Hua; Acta Crystallographica Section C 69 (2013) 494–497; doi:10.1107/S0108270113010007

data_2018949
_publ_section_title
;
 Poly[bis(\m-5-iodoisophthalato)(methanol)dilead(II)] exhibiting a novel
 centrosymmetric rhombus-shaped I~4~ unit
;
_journal_coeditor_code           EM3057
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              494
_journal_page_last               497
_journal_paper_doi               10.1107/S0108270113010007
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '[Pb2 (C8 H3 I O4)2 (C H4 O)]'
_chemical_formula_moiety         'C17 H10 I2 O9 Pb2'
_chemical_formula_sum            'C17 H10 I2 O9 Pb2'
_chemical_formula_weight         1026.43
_chemical_name_systematic
;
Poly[bis(\m-5-iodoisophthalato)(methanol)dilead(II)]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.8970(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   4.3137(4)
_cell_length_b                   27.918(2)
_cell_length_c                   17.6437(15)
_cell_measurement_reflns_used    7918
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.478
_cell_measurement_theta_min      2.314
_cell_volume                     2119.9(3)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_molecular_graphics    'SHELXTL-Plus (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker--Nonius KappaCCD'
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_av_sigmaI/netI    0.0376
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18249
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.46
_exptl_absorpt_coefficient_mu    18.822
_exptl_absorpt_correction_T_max  0.1100
_exptl_absorpt_correction_T_min  0.0583
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Bruker, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.216
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1816
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_refine_diff_density_max         2.225
_refine_diff_density_min         -1.647
_refine_ls_extinction_coef       0.00024(4)
_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   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         4855
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0318
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0209P)^2^+11.2420P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0681
_refine_ls_wR_factor_ref         0.0701
_reflns_number_gt                4302
_reflns_number_total             4855
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            em3057.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2018949
_cod_database_fobs_code          2018949