Synthesis and structures of two new 12-member ring crown-shaped oxovanadium borophosphates
Zhao, Yongnan; Zhu, Guangshan; Liu, Wang; Zou, Yongcun; Pang, Wenqin; Chemical Communications  (1999) 2219–; doi:10.1039/a906668c

data_7110695
_publ_section_title
;
 Synthesis and structures of two new 12-member ring crown-shaped
 oxovanadium borophosphates
;
_journal_issue                   21
_journal_name_full               'Chemical Communications'
_journal_page_first              2219
_journal_paper_doi               10.1039/a906668c
_journal_year                    1999
_chemical_formula_sum            'C24 H120 B6 N17 O86 P12 V12'
_chemical_formula_weight         3071.15
_chemical_name_common            vbp-j1
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                   21.454(11)
_cell_length_b                   16.315(6)
_cell_length_c                   29.651(12)
_cell_measurement_reflns_used    190
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.3
_cell_measurement_theta_min      1.67
_cell_volume                     10379(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    SHELXP-97
_computing_publication_material  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 0.929
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measurement_device_type  'Bruker CCD area detector '
_diffrn_measurement_method       'phi and omega 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  0.0638
_diffrn_reflns_av_sigmaI/netI    0.0942
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            20909
_diffrn_reflns_theta_full        23.23
_diffrn_reflns_theta_max         23.23
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    1.343
_exptl_absorpt_correction_T_max  0.9333
_exptl_absorpt_correction_T_min  0.8130
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.966
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombic
_exptl_crystal_F_000             6228
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.294
_refine_diff_density_min         -0.647
_refine_diff_density_rms         0.130
_refine_ls_extinction_coef       0.00000(6)
_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   0.840
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     784
_refine_ls_number_reflns         6902
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      0.847
_refine_ls_R_factor_all          0.1014
_refine_ls_R_factor_gt           0.0586
_refine_ls_shift/su_max          4.765
_refine_ls_shift/su_mean         0.152
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1411P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1708
_refine_ls_wR_factor_ref         0.1901
_reflns_number_gt                4099
_reflns_number_total             6902
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            906668csup1.cif
_cod_data_source_block           vbp-j1
_cod_original_cell_volume        10378(8)
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               7110695