Synthesis and Structure of Bismuth(III)-Containing Noncentrosymmetric Phosphates, Cs3KBi2M4(PO4)6Cl (M = Mn, Fe). Monoclinic (Cc) and Tetragonal (P43) Polymorphs Templated by Chlorine-Centered Cl(Bi2Cs) Acentric Units
J. Palmer West; Dino Sulejmanovic; Shiou-Jyh Hwu; Jian He; Don VanDerveer; B. Keith Johnson; Inorganic Chemistry 51 (2012) 9723–9729; doi:10.1021/ic3010129

data_4330344
_publ_contact_author_address
;Department of Chemistry
Clemson University
Clemson, SC  29634-0973 
USA
;
_publ_contact_author_email       shwu@clemson.edu
_publ_contact_author_name        'Shiou-Jyh Hwu'
_publ_contact_author_phone       864-656-5031
_publ_section_title
;
 Synthesis and Structure of Bismuth(III)-Containing Noncentrosymmetric
 Phosphates, Cs3KBi2M4(PO4)6Cl (M = Mn, Fe). Monoclinic (Cc) and
 Tetragonal (P43) Polymorphs Templated by Chlorine-Centered Cl(Bi2Cs)
 Acentric Units
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9723
_journal_page_last               9729
_journal_paper_doi               10.1021/ic3010129
_journal_volume                  51
_journal_year                    2012
_chemical_absolute_configuration unk
_chemical_formula_sum            'Bi2 Cl Cs3 K Mn4 O24 P6'
_chemical_formula_weight         1680.82
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           78
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4cw'
_symmetry_space_group_name_H-M   'P 43'
_atom_sites_solution_hydrogens   none
_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                   12.2098(17)
_cell_length_b                   12.2098(17)
_cell_length_c                   17.848(4)
_cell_measurement_reflns_used    4689
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.02
_cell_volume                     2660.8(8)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_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  0.0747
_diffrn_reflns_av_sigmaI/netI    0.0617
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            22984
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    19.782
_exptl_absorpt_correction_T_max  0.2000
_exptl_absorpt_correction_T_min  0.1170
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB, CrystalClear'
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    4.196
_exptl_crystal_description       chunk
_exptl_crystal_F_000             2996
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.14
_refine_diff_density_max         3.034
_refine_diff_density_min         -2.026
_refine_diff_density_rms         0.328
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.013(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         4689
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0528
_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^)+(0.0672P)^2^+11.0070P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1335
_refine_ls_wR_factor_ref         0.1380
_reflns_number_gt                4370
_reflns_number_total             4689
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3010129_si_003_2.cif
_cod_data_source_block           beta-Cs3KBi2Mn4(PO4)6Cl
_cod_original_cell_volume        2660.7(8)
_cod_database_code               4330344