Three new high-nuclear transition-metal-substituted heteropolytungstates: syntheses, crystal structures, magnetic studies and NLO properties.
Luo, Xi-Ming; Chen, Lu; Dong, Ya-Yu; Li, Jing; Cui, Chen-Hui; Cao, Jia-Peng; Xu, Yan; Dalton transactions (Cambridge, England : 2003) 47 (2018) 9504–9511; doi:10.1039/c8dt01613e

data_7046833
_publ_section_title
;
 Three new high-nuclear transition-metal-substituted heteropolytungstates:
 syntheses, crystal structures, magnetic studies and NLO properties.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9504
_journal_page_last               9511
_journal_paper_doi               10.1039/c8dt01613e
_journal_volume                  47
_journal_year                    2018
_chemical_formula_sum            'C24 H94 N10 Ni13 O96 Si2 W18'
_chemical_formula_weight         6187.80
_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
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-06-19 deposited with the CCDC.
2018-06-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.383(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.476(2)
_cell_length_b                   18.886(2)
_cell_length_c                   20.8900(19)
_cell_measurement_reflns_used    7849
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.2
_cell_measurement_theta_min      2.271
_cell_volume                     11973.3(18)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker Apex2 CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0611
_diffrn_reflns_av_unetI/netI     0.0543
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            43210
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.499
_diffrn_reflns_theta_min         1.270
_exptl_absorpt_coefficient_mu    19.326
_exptl_absorpt_correction_T_max  0.248
_exptl_absorpt_correction_T_min  0.205
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    3.433
_exptl_crystal_description       block-shaped
_exptl_crystal_F_000             11200
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         3.089
_refine_diff_density_min         -2.489
_refine_diff_density_rms         0.291
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     784
_refine_ls_number_reflns         11103
_refine_ls_number_restraints     276
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0369
_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^)+(0.0477P)^2^+71.7028P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0952
_refine_ls_wR_factor_ref         0.1016
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8723
_reflns_number_total             11103
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01613e2.cif
_cod_data_source_block           a01
_cod_depositor_comments
'Adding full bibliography for 7046833--7046835.cif.'
_cod_original_cell_volume        11973(2)
_cod_database_code               7046833
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.205
_shelx_estimated_absorpt_t_max   0.248
_shelx_res_checksum              96760