Syntheses, structures and magnetic properties of two unprecedented hybrid compounds constructed from open Wells-Dawson anions and high-nuclear transition metal clusters.
Guo, Jiuyu; Zhang, Deng; Chen, Lei; Song, You; Zhu, Dunru; Xu, Yan; Dalton transactions (Cambridge, England : 2003) 42 (2013) 8454–8459; doi:10.1039/c3dt50155h

data_7022850
_publ_section_title
;
 Syntheses, structures and magnetic properties of two unprecedented hybrid
 compounds constructed from open Wells-Dawson anions and high-nuclear
 transition metal clusters.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8454
_journal_page_last               8459
_journal_paper_doi               10.1039/c3dt50155h
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety
Na2(C3N2H12)4{[Ni5(OH)3(H2O)4(CH3CO2)][SiW9O33]2}.12.5H2O
_chemical_formula_sum            'C14 H87 N8 Na2 Ni5 O87.5 Si2 W18'
_chemical_formula_weight         5472.91
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.906(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.2098(18)
_cell_length_b                   18.524(3)
_cell_length_c                   35.750(5)
_cell_measurement_reflns_used    7788
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.9865
_cell_measurement_theta_min      2.2795
_cell_volume                     8702(2)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0928
_diffrn_reflns_av_unetI/netI     0.0832
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            61910
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.15
_exptl_absorpt_coefficient_mu    24.902
_exptl_absorpt_correction_T_max  0.1541
_exptl_absorpt_correction_T_min  0.1089
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    4.174
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'square sheet'
_exptl_crystal_F_000             9776
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.912
_refine_diff_density_min         -1.979
_refine_diff_density_rms         0.404
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1240
_refine_ls_number_reflns         16098
_refine_ls_number_restraints     116
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0783
_refine_ls_R_factor_gt           0.0423
_refine_ls_shift/su_max          0.037
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0380P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0825
_refine_ls_wR_factor_ref         0.0967
_reflns_number_gt                11193
_reflns_number_total             16098
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt50155h.txt
_cod_data_source_block           gjy-35
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        8701(2)
_cod_original_sg_symbol_H-M      'P2(1)/c '
_cod_original_formula_sum        'C14 H87 N8 Na2 Ni5 O87.50 Si2 W18'
_cod_database_code               7022850