Two synthetic routes generate two isopolyoxoniobates based on {Nb16} and {Nb20}
Niu, Jingyang; Liang, Zhijie; Qiao, Yuanyuan; Li, Miaomiao; Ma, Pengtao; Wang, Jingping; Dalton Transactions  (2019) –; doi:10.1039/C9DT04147H

data_7701994
_publ_section_title
;
 Two synthetic routes generate two isopolyoxoniobates based on {Nb16} and
 {Nb20}
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT04147H
_journal_year                    2019
_chemical_formula_moiety
'0.5(C120 H126 Cu12 K6 N24 Nb32 O110), 40(H2O)'
_chemical_formula_sum            'C60 H143 Cu6 K3 N12 Nb16 O95'
_chemical_formula_weight         4537.96
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-11-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-11-18 deposited with the CCDC.	2019-11-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 118.3019(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.7006(16)
_cell_length_b                   24.1052(17)
_cell_length_c                   24.8467(16)
_cell_measurement_reflns_used    3730
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.95
_cell_measurement_theta_min      2.36
_cell_volume                     13025.6(15)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Helios multilayer optic'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0697
_diffrn_reflns_av_unetI/netI     0.0834
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            33863
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.100
_diffrn_reflns_theta_max         25.100
_diffrn_reflns_theta_min         1.261
_diffrn_source_type              Microfocus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.518
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5810
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    2.314
_exptl_crystal_description       block
_exptl_crystal_F_000             8936
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.665
_refine_diff_density_min         -0.781
_refine_diff_density_rms         0.205
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     703
_refine_ls_number_reflns         11621
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0900
_refine_ls_R_factor_gt           0.0542
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0898P)^2^+42.8065P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1487
_refine_ls_wR_factor_ref         0.1755
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7685
_reflns_number_total             11621
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04147h2.cif
_cod_data_source_block           1
_cod_database_code               7701994
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.660
_shelx_estimated_absorpt_t_min   0.529
_diffrn_source_source            'Incoatc Ius 3.0 '
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3. Others
 Fixed Sof: K2(0.5) O11W(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C13(H13), C14(H14), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21),
  C22(H22), C23(H23), C24(H24), C27(H27), C28(H28), C29(H29), C30(H30)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 1042.0 electrons were found in a volume of 2147.9\%A^3 in void. This is consistent with the presence of 26[H2O] per formula unit which account for 1040.0 electrons.
;
_shelx_res_checksum              44279
_shelx_fab_checksum              31137
_olex2_submission_special_instructions 'No special instructions were received'