Syntheses, structures and properties of three organic‒inorganic hybrid polyoxotungstates constructed from {Ni6PW9} building blocks: from isolated clusters to 2-D layers
Zhang, Zhong; Wang, Yue-Lin; Li, Hai-Lou; Sun, Ke-Ning; Yang, Guo-Yu; CrystEngComm 21 (2019) 2641–; doi:10.1039/C9CE00194H

data_7232486
_publ_section_title
;
 Syntheses, structures and properties of three organic--inorganic hybrid
 polyoxotungstates constructed from {Ni6PW9} building blocks: from
 isolated clusters to 2-D layers
;
_journal_issue                   16
_journal_name_full               CrystEngComm
_journal_page_first              2641
_journal_paper_doi               10.1039/C9CE00194H
_journal_volume                  21
_journal_year                    2019
_chemical_formula_sum            'C18 H67 N10 Ni7 O53 P W9'
_chemical_formula_weight         3368.40
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2018-09-21 deposited with the CCDC.    2019-03-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3441(3)
_cell_length_b                   14.2773(3)
_cell_length_c                   36.0138(11)
_cell_measurement_temperature    293(2)
_cell_volume                     6861.3(3)
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0475
_diffrn_reflns_av_unetI/netI     0.0647
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            28423
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.006
_diffrn_reflns_theta_max         25.006
_diffrn_reflns_theta_min         2.853
_exptl_absorpt_coefficient_mu    17.021
_exptl_crystal_density_diffrn    3.261
_exptl_crystal_F_000             6184
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.100
_refine_diff_density_max         2.179
_refine_diff_density_min         -1.780
_refine_diff_density_rms         0.304
_refine_ls_abs_structure_details
;
 Flack x determined using 4225 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.382(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     883
_refine_ls_number_reflns         12000
_refine_ls_number_restraints     171
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0510
_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^)+(0.0461P)^2^+162.9642P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1105
_refine_ls_wR_factor_ref         0.1137
_reflns_Friedel_coverage         0.800
_reflns_Friedel_fraction_full    0.987
_reflns_Friedel_fraction_max     0.987
_reflns_number_gt                11078
_reflns_number_total             12000
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce00194h1.cif
_cod_data_source_block           1_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7232485--7232487.cif.'
_cod_database_code               7232486
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.150
_shelx_estimated_absorpt_t_max   0.281
_shelx_res_checksum              31376