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_7022851
_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
(C3N2H12)4{[Co6(OH)5(H2O)2(CH3CO2)][HSiW9O33]2}.6H2O
_chemical_formula_sum            'C14 H74 Co6 N8 O81 Si2 W18'
_chemical_formula_weight         5369.85
_chemical_name_systematic
;
?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 90.188(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.645(3)
_cell_length_b                   19.187(5)
_cell_length_c                   19.060(5)
_cell_measurement_reflns_used    14562
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.6105
_cell_measurement_theta_min      2.2045
_cell_volume                     4624(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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0481
_diffrn_reflns_av_unetI/netI     0.0543
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            33946
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.07
_exptl_absorpt_coefficient_mu    23.463
_exptl_absorpt_correction_T_max  0.1651
_exptl_absorpt_correction_T_min  0.1172
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            Pink
_exptl_crystal_density_diffrn    3.853
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'square sheet'
_exptl_crystal_F_000             4758
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.869
_refine_diff_density_min         -1.517
_refine_diff_density_rms         0.265
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.015(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1171
_refine_ls_number_reflns         16803
_refine_ls_number_restraints     126
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0325
_refine_ls_shift/su_max          0.039
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0461P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0804
_refine_ls_wR_factor_ref         0.0833
_reflns_number_gt                15551
_reflns_number_total             16803
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt50155h.txt
_cod_data_source_block           gjy-31
_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        4624.2(19)
_cod_original_sg_symbol_H-M      'P2(1) '
_cod_database_code               7022851