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_7110696
_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            'C28 H128 B6 K N20 O84 P12 V12'
_chemical_formula_weight         3176.38
_chemical_name_common            vbp-j2
_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                   21.537(2)
_cell_length_b                   16.2667(13)
_cell_length_c                   29.717(4)
_cell_measurement_reflns_used    150
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.3
_cell_measurement_theta_min      1.67
_cell_volume                     10410.9(19)
_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 0.980
_diffrn_measured_fraction_theta_max 0.980
_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  0.0945
_diffrn_reflns_av_sigmaI/netI    0.0758
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            20918
_diffrn_reflns_theta_full        23.29
_diffrn_reflns_theta_max         23.29
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    1.381
_exptl_absorpt_correction_T_max  0.9205
_exptl_absorpt_correction_T_min  0.7820
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.027
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombic
_exptl_crystal_F_000             6452
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.749
_refine_diff_density_min         -0.648
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.950
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     759
_refine_ls_number_reflns         7345
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.950
_refine_ls_R_factor_all          0.0839
_refine_ls_R_factor_gt           0.0576
_refine_ls_shift/su_max          3.199
_refine_ls_shift/su_mean         0.104
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1056P)^2^+41.3646P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1540
_refine_ls_wR_factor_ref         0.1754
_reflns_number_gt                5235
_reflns_number_total             7345
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            906668csup1.cif
_cod_data_source_block           vbp-j2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' tag value 'orthrombic' was replaced with
'orthorhombic' value as specified in the replacement file
'/home/robertas/cod-tools/perl-scripts/inputs/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        10410.8(18)
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               7110696