A spherical deca-vanadophosphate covalent assembled all-inorganic open framework.
Hu, Hailiang; Guo, Zhenyu; Li, Kaixuan; Lin, Xiaoling; Liu, Yang; Kang, Zhenhui; Dalton transactions (Cambridge, England : 2003) 46 (2017) 3115–3119; doi:10.1039/c6dt03850f

data_7041741
_publ_section_title
;
 A spherical deca-vanadophosphate covalent assembled all-inorganic open
 framework.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3115
_journal_page_last               3119
_journal_paper_doi               10.1039/c6dt03850f
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety
'0.5(O102 P12 V30), 8(H0.5 O0.25), 1(O), 12(H3 N0.75)'
_chemical_formula_sum            'H42 N9 O54 P6 V15'
_chemical_formula_weight         1982.34
_space_group_crystal_system      cubic
_space_group_IT_number           229
_space_group_name_Hall           '-I 4 2 3'
_space_group_name_H-M_alt        'I m -3 m'
_symmetry_space_group_name_Hall  '-I 4 2 3'
_symmetry_space_group_name_H-M   'I m -3 m'
_atom_sites_solution_hydrogens   difmap
_audit_creation_date             2017-01-15
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5289)
;
_audit_update_record
;
2017-01-16 deposited with the CCDC.
2017-01-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.0271(5)
_cell_length_b                   16.0271(5)
_cell_length_c                   16.0271(5)
_cell_measurement_reflns_used    3554
_cell_measurement_temperature    298
_cell_measurement_theta_max      27.442
_cell_measurement_theta_min      2.542
_cell_volume                     4116.8(2)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      298.0
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_unetI/netI     0.0104
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13392
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.442
_diffrn_reflns_theta_min         5.398
_exptl_absorpt_coefficient_mu    1.818
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.599
_exptl_crystal_description       block
_exptl_crystal_F_000             1944
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.408
_refine_diff_density_min         -0.702
_refine_diff_density_rms         0.172
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.164
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     48
_refine_ls_number_reflns         495
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.153
_refine_ls_R_factor_all          0.0881
_refine_ls_R_factor_gt           0.0842
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1469P)^2^+43.9141P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2524
_refine_ls_wR_factor_ref         0.2560
_reflns_Friedel_coverage         0.000
_reflns_number_gt                457
_reflns_number_total             495
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt03850f2.cif
_cod_data_source_block           1
_cod_depositor_comments          'Adding full bibliography for 7041741.cif.'
_cod_original_cell_volume        4116.8(4)
_cod_database_code               7041741
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All N(H,H,H) groups, All O(H) groups
2. Restrained distances
 V2-O2
 2 with sigma of 0.02
 V1-O2
 2 with sigma of 0.02
 O3-V2
 1.6 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O2W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O1W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: V1(0.0625) V2(0.25) O1(0.0625) O2(0.25) O3(0.25) O1W(0.04167)
 H1W(0.08334) O2W(0.02083) N1(0.1875) H1A(0.1875) H1B(0.1875) H1C(0.375)
 Fixed X: O1W(0.25)
 Fixed Y: O1W(0.75)
 Fixed Z: O1W(0.75)
5.a Riding coordinates:
 O1W(H1W), N1(H1A,H1B,H1C)
;
_shelx_res_checksum              46556
_olex2_submission_special_instructions 'No special instructions were received'