3D-transition metal mono-substituted Keggin polyoxotungstate with an antenna molecule: synthesis, structure and characterization
Liu, Hongsheng; Gómez-García, Carlos J.; Peng, Jun; Sha, Jingquan; Li, Yangguang; Yan, Yechao; Dalton Transactions  (2008) 6211–6218; doi:10.1039/b805714a

data_7004333
_publ_section_title
;
 3D-transition metal mono-substituted Keggin polyoxotungstate with an
 antenna molecule: synthesis, structure and characterization
;
_journal_issue                   44
_journal_name_full               'Dalton Transactions'
_journal_page_first              6211
_journal_page_last               6218
_journal_paper_doi               10.1039/b805714a
_journal_year                    2008
_chemical_formula_sum            'C20.4 H47.6 N13.6 Ni O46.2 Si W11'
_chemical_formula_weight         3331.87
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                82.21(3)
_cell_angle_beta                 77.22(3)
_cell_angle_gamma                70.75(3)
_cell_formula_units_Z            2
_cell_length_a                   12.117(2)
_cell_length_b                   12.745(3)
_cell_length_c                   21.917(4)
_cell_measurement_temperature    466(2)
_cell_volume                     3109.1(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      273(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'CCDC area detector'
_diffrn_measurement_method       'phi and omega 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  0.0292
_diffrn_reflns_av_sigmaI/netI    0.0643
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            16183
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    20.683
_exptl_absorpt_correction_T_max  0.2315
_exptl_absorpt_correction_T_min  0.0787
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            blue-green
_exptl_crystal_density_diffrn    3.559
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       sheet-like
_exptl_crystal_F_000             2982
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         4.580
_refine_diff_density_min         -2.188
_refine_diff_density_rms         0.440
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     809
_refine_ls_number_reflns         10948
_refine_ls_number_restraints     191
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0806
_refine_ls_R_factor_gt           0.0663
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0514P)^2^+162.3112P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1474
_refine_ls_wR_factor_ref         0.1533
_reflns_number_gt                9198
_reflns_number_total             10948
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b805714a.txt
_cod_data_source_block           ch1
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        3109.0(11)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C20.40 H47.60 N13.60 Ni O46.20 Si W11'
_cod_database_code               7004333