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_4325705
_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         'C36 H52 N6 O8 P2 Sb3, 1.5(C7 H8), H2 O'
_chemical_formula_sum            'C46.5 H66 N6 O9 P2 Sb3'
_chemical_formula_weight         1280.24
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                71.582(7)
_cell_angle_beta                 85.124(6)
_cell_angle_gamma                66.051(5)
_cell_formula_units_Z            2
_cell_length_a                   12.2120(8)
_cell_length_b                   13.6871(10)
_cell_length_c                   18.4900(9)
_cell_measurement_reflns_used    53043
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     2676.5(3)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0463
_diffrn_reflns_av_sigmaI/netI    0.0343
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            52950
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.75
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.619
_exptl_absorpt_correction_T_max  0.843
_exptl_absorpt_correction_T_min  0.661
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_description       plate
_exptl_crystal_F_000             1284
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.14
_platon_squeeze_details
;
;
_refine_diff_density_max         1.326
_refine_diff_density_min         -1.178
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     475
_refine_ls_number_reflns         12239
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0309
_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^)+(0.0229P)^2^+5.2666P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0640
_refine_ls_wR_factor_ref         0.0679
_reflns_number_gt                10318
_reflns_number_total             12239
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2009144_si_001.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        2676.4(3)
_cod_original_formula_sum        'C46.50 H66 N6 O9 P2 Sb3'
_cod_database_code               4325705