Keggin unit supported transition metal complexes: hydrothermal synthesis and characterization of [Ni(2,2′-bipy)3]1.5[PW12O40Ni(2,2′-bipy)2(H2O)]·0.5H2O and [Co(1,10′-phen)3]1.5[PMo12O40Co(1,10′-phen)2(H2O)]·0.5H2O
Xu, Yan; Zhang, Kou-Lin; Zhang, Yong; You, Xiao-Zeng; Xu, Ji-Qing; Chemical Communications  (2000) 153–; doi:10.1039/a908527k

data_7110776
_publ_section_title
;
 Keggin unit supported transition metal complexes: hydrothermal synthesis
 and characterization of
 [Ni(2,2&#x2032;-bipy)3]1.5[PW12O40Ni(2,2&#x2032;-bipy)2(H2O)]&#x00B7;0.5H2O
 and
 [Co(1,10&#x2032;-phen)3]1.5[PMo12O40Co(1,10&#x2032;-phen)2(H2O)]&#x00B7;0.5H2O
;
_journal_issue                   2
_journal_name_full               'Chemical Communications'
_journal_page_first              153
_journal_paper_doi               10.1039/a908527k
_journal_year                    2000
_chemical_formula_sum            'C65 H68 N13 Ni2.5 O41.5 P W12'
_chemical_formula_weight         4079.27
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.21(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   46.768(9)
_cell_length_b                   14.340(3)
_cell_length_c                   25.945(5)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      5.62
_cell_measurement_theta_min      1.53
_cell_volume                     17400(6)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '2\q/\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  0.0305
_diffrn_reflns_av_sigmaI/netI    0.0900
_diffrn_reflns_limit_h_max       51
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            14314
_diffrn_reflns_theta_max         23.02
_diffrn_reflns_theta_min         1.57
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    16.434
_exptl_absorpt_correction_T_max  0.0729
_exptl_absorpt_correction_T_min  0.0239
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    3.114
_exptl_crystal_description       block
_exptl_crystal_F_000             14832
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.20
_refine_diff_density_max         3.900
_refine_diff_density_min         -4.060
_refine_diff_density_rms         0.501
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.033
_refine_ls_goodness_of_fit_obs   1.216
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     891
_refine_ls_number_reflns         12113
_refine_ls_number_restraints     421
_refine_ls_restrained_S_all      1.034
_refine_ls_restrained_S_obs      1.190
_refine_ls_R_factor_all          0.1067
_refine_ls_R_factor_obs          0.0732
_refine_ls_shift/esd_max         -0.650
_refine_ls_shift/esd_mean        0.020
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1100P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1984
_refine_ls_wR_factor_obs         0.1827
_reflns_number_observed          7834
_reflns_number_total             12121
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            a908527ksup1.cif
_cod_data_source_block           f068
_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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1100P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1100P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        17400.0(61)
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C65 H68 N13 Ni2.50 O41.50 P W12'
_cod_database_code               7110776