NCN-Chelated Organoantimony(III) and Organobismuth(III) Phosphates: Synthesis and Solid-State and Solution Structures
Tomáš Svoboda; Libor Dostál; Roman Jambor; Aleš Růžička; Robert Jirásko; Antonín Lyčka; Inorganic Chemistry 50 (2011) 6411–6413; doi:10.1021/ic2009144

data_4325706
_publ_section_title
;
 NCN-Chelated Organoantimony(III) and Organobismuth(III) Phosphates:
 Synthesis and Solid-State and Solution Structures
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6411
_journal_page_last               6413
_journal_paper_doi               10.1021/ic2009144
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C39 H67 Cl6 N6 O10 P2 Sb3'
_chemical_formula_sum            'C39 H67 Cl6 N6 O10 P2 Sb3'
_chemical_formula_weight         1419.88
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           55
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2 2ab'
_symmetry_space_group_name_H-M   'P b a 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
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.4370(8)
_cell_length_b                   24.8581(19)
_cell_length_c                   11.1430(2)
_cell_measurement_reflns_used    39345
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     5660.9(5)
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_collection
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_data_reduction        'COLLECT and DENZO'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150(1)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker Nonius KappaCCD area detector'
_diffrn_measurement_method       '\f and \w scans to fill the Ewald sphere'
_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  0.0548
_diffrn_reflns_av_sigmaI/netI    0.0314
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            38656
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.92
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.815
_exptl_absorpt_correction_T_max  0.754
_exptl_absorpt_correction_T_min  0.652
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.666
_exptl_crystal_description       block
_exptl_crystal_F_000             2832
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.27
_platon_squeeze_details
;
;
_refine_diff_density_max         3.844
_refine_diff_density_min         -3.838
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         6784
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0440
_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^)+(0.0321P)^2^+42.3212P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0973
_refine_ls_wR_factor_ref         0.1024
_reflns_number_gt                5873
_reflns_number_total             6734
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2009144_si_002.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        5660.9(6)
_cod_database_code               4325706