Synthesis and Molecular Structure of a Water-Soluble, Dimeric Tri-Titanium(IV)-Substituted Wells-Dawson Polyoxometalate Containing Two Bridging (C5Me5)Rh2+ Groups.
Matsuki, Yusuke; Hoshino, Takahiro; Takaku, Shoko; Matsunaga, Satoshi; Nomiya, Kenji; Inorganic chemistry 54 (2015) 11105–11113; doi:10.1021/acs.inorgchem.5b01206

data_4346284
_publ_section_title
;
 Synthesis and Molecular Structure of a Water-Soluble, Dimeric
 Tri-Titanium(IV)-Substituted Wells-Dawson Polyoxometalate Containing Two
 Bridging (C5Me5)Rh2+ Groups.
;
_journal_issue                   23
_journal_name_full               'Inorganic chemistry'
_journal_page_first              11105
_journal_page_last               11113
_journal_paper_doi               10.1021/acs.inorgchem.5b01206
_journal_volume                  54
_journal_year                    2015
_chemical_formula_sum            'C20 H30 K8 Na0 O176 P4 Rh2 Ti6 W30'
_chemical_formula_weight         9531.84
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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                105.7400(10)
_cell_angle_beta                 90.6940(10)
_cell_angle_gamma                90.5890(10)
_cell_formula_units_Z            1
_cell_length_a                   14.3212(14)
_cell_length_b                   15.4969(15)
_cell_length_c                   21.536(2)
_cell_measurement_reflns_used    8110
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.24
_cell_measurement_theta_min      2.38
_cell_volume                     4599.6(8)
_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      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'CCD 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  0.0387
_diffrn_reflns_av_sigmaI/netI    0.0484
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            54500
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    19.418
_exptl_absorpt_correction_T_max  0.3057
_exptl_absorpt_correction_T_min  0.1058
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    3.441
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4212
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         7.409
_refine_diff_density_min         -2.005
_refine_diff_density_rms         0.373
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     969
_refine_ls_number_reflns         20878
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0433
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0494P)^2^+136.1118P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1128
_refine_ls_wR_factor_ref         0.1185
_reflns_number_gt                17340
_reflns_number_total             20878
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b01206_si_002.cif
_cod_data_source_block           yma056
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        4599.5(8)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4346284