Synthesis and Modular Structural Architectures of Mineralogically Inspired Novel Complex Pb Oxyhalides
Oleg I. Siidra; Diana O. Zinyakhina; Anastasiya I. Zadoya; Sergey V. Krivovichev; Rick W. Turner; Inorganic Chemistry 52 (2013) 12799–12805; doi:10.1021/ic402066h

data_4336645
_publ_section_title
;
 Synthesis and Modular Structural Architectures of Mineralogically
 Inspired Novel Complex Pb Oxyhalides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12799
_journal_page_last               12805
_journal_paper_doi               10.1021/ic402066h
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'Cl0.5 O3 Pb2.75 Si0.25'
_chemical_formula_weight         642.52
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           87
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4'
_symmetry_space_group_name_H-M   'I 4/m'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   3.8890(7)
_cell_length_b                   3.8890(7)
_cell_length_c                   32.560(6)
_cell_measurement_temperature    296(2)
_cell_volume                     492.45(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0431
_diffrn_reflns_av_sigmaI/netI    0.0294
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            2085
_diffrn_reflns_theta_full        27.90
_diffrn_reflns_theta_max         27.90
_diffrn_reflns_theta_min         2.50
_exptl_absorpt_coefficient_mu    94.011
_exptl_crystal_density_diffrn    8.666
_exptl_crystal_F_000             1046
_refine_diff_density_max         5.504
_refine_diff_density_min         -3.182
_refine_diff_density_rms         0.755
_refine_ls_extinction_coef       0.0030(5)
_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   1.177
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     30
_refine_ls_number_reflns         315
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.177
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0518
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0778P)^2^+47.1450P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1391
_refine_ls_wR_factor_ref         0.1418
_reflns_number_gt                296
_reflns_number_total             315
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic402066h_si_001_3.cif
_cod_data_source_block           Pb5.5Si0.5O6Cl_(compound_3)
_cod_original_formula_sum        'Cl0.50 O3 Pb2.75 Si0.25'
_cod_database_code               4336645