Rhodium Derivatives of Lacunary Heteropolytungstates Illustrate Metalloporphyrin Analogies. Reductive Dimerization to Rh2-Linked Keggin Moieties
Xinyi Wei; Robert E. Bachman; Michael T. Pope; Journal of the American Chemical Society 120 (1998) 10248–10253; doi:10.1021/ja981066l

data_4116842
_publ_section_title
;
 Rhodium Derivatives of Lacunary Heteropolytungstates Illustrate
 Metalloporphyrin Analogies. Reductive Dimerization to Rh2-Linked Keggin
 Moieties
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10248
_journal_page_last               10253
_journal_paper_doi               10.1021/ja981066l
_journal_volume                  120
_journal_year                    1998
_chemical_formula_sum            'K9.5 O88 P2 Rh2 W22'
_chemical_formula_weight         6091.91
_chemical_name_systematic
; 

 ? 

;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                96.56(2)
_cell_angle_beta                 97.12(2)
_cell_angle_gamma                91.318(13)
_cell_formula_units_Z            2
_cell_length_a                   12.703(6)
_cell_length_b                   17.868(8)
_cell_length_c                   19.131(9)
_cell_measurement_temperature    173(2)
_cell_volume                     4278(3)
_computing_cell_refinement       'Siemens SMART/SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Siemens SMART 1K CCD'
_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  0.3715
_diffrn_reflns_av_sigmaI/netI    0.2791
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            39301
_diffrn_reflns_theta_max         23.13
_diffrn_reflns_theta_min         1.15
_exptl_absorpt_coefficient_mu    30.430
_exptl_absorpt_correction_T_max  0.11062
_exptl_absorpt_correction_T_min  0.03169
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    4.730
_exptl_crystal_description       plate
_exptl_crystal_F_000             5265
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         9.860
_refine_diff_density_min         -9.929
_refine_diff_density_rms         1.496
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.168
_refine_ls_goodness_of_fit_obs   1.269
_refine_ls_matrix_type           full
_refine_ls_number_parameters     528
_refine_ls_number_reflns         11812
_refine_ls_number_restraints     144
_refine_ls_restrained_S_all      1.202
_refine_ls_restrained_S_obs      1.308
_refine_ls_R_factor_all          0.2907
_refine_ls_R_factor_obs          0.1831
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1844P)^2^+6056.5410P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.5251
_refine_ls_wR_factor_obs         0.4182
_reflns_number_observed          6089
_reflns_number_total             19186
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja981066l.cif
_cod_data_source_block           merabr
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1844P)^2^+6056.5410P] 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^)+(0.1844P)^2^+6056.5410P] 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        4277.6(33)
_cod_original_formula_sum        'K9.50 O88 P2 Rh2 W22'
_cod_database_code               4116842