A new redox-based and stepwise synthetic strategy lead to an unprecedented mixed-valence Keggin-type tungstovanadophosphate (WVI/VIV) bi-capped by vanadium(VIII)-complexes
Chen, Wu-Hua; Lai, Yu-Zhen; Hu, Zhi-Biao; Liu, Jin-Xian; Guo, Xiang-Guang; Yuan, Qiu-Lan; Zhao, Jin-Hua; Mi, Jin-Xiao; Luo, Jiang-Shui; New Journal of Chemistry 42 (2018) 8738–; doi:10.1039/C8NJ00714D

data_7057256
_publ_section_title
;
 A new redox-based and stepwise synthetic strategy lead to an
 unprecedented mixed-valence Keggin-type tungstovanadophosphate (WVI/VIV)
 bi-capped by vanadium(VIII)-complexes
;
_journal_issue                   11
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              8738
_journal_paper_doi               10.1039/C8NJ00714D
_journal_volume                  42
_journal_year                    2018
_chemical_formula_moiety
'C16 H48 N12 Na O80 P2 V12 W16, 2(O), 4(C4 H16 N3)'
_chemical_formula_sum            'C32 H116 N24 Na O82 P2 V12 W16'
_chemical_formula_weight         5787.29
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-05-14
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-10-18 deposited with the CCDC.
2018-04-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.728(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.8135(5)
_cell_length_b                   13.0499(3)
_cell_length_c                   37.5978(7)
_cell_measurement_reflns_used    9372
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      3.2
_cell_volume                     10666.3(4)
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku R-axis Spider'
_diffrn_measurement_method       '\w oscillation'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0504
_diffrn_reflns_av_unetI/netI     0.0698
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            25850
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         3.222
_exptl_absorpt_coefficient_mu    18.320
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    3.604
_exptl_crystal_description       block
_exptl_crystal_F_000             10532
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_exptl_transmission_factor_max   0.092
_exptl_transmission_factor_min   0.026
_refine_diff_density_max         1.999
_refine_diff_density_min         -2.515
_refine_diff_density_rms         0.316
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     718
_refine_ls_number_reflns         9372
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0467
_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^)+(0.0082P)^2^+55.1826P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0691
_refine_ls_wR_factor_ref         0.0733
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7667
_reflns_number_total             9372
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj00714d2.cif
_cod_data_source_block           1
_cod_depositor_comments          'Adding full bibliography for 7057256.cif.'
_cod_database_code               7057256
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups, All N(H,H) groups, All N(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 N2(H2), N5(H5)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), N1(H1C,H1D), N3(H3C,H3D), C5(H5A,H5B),
 C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), N4(H4A,H4B), N6(H6C,H6D), C9(H9A,H9B),
 C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), N8(H8C,H8D), C13(H13A,H13B),
 C14(H14A,H14B), N10(H10C,H10D), C15(H15A,H15B), C16(H16A,H16B)
2.c Idealised Me refined as rotating group:
 N7(H7C,H7D,H7E), N9(H9C,H9D,H9E), N11(H11C,H11D,H11E), N12(H12C,H12D,H12E)
;
_olex2_submission_special_instructions 'No special instructions were received'