Rhodium-Carbon Bond Formation in Aqueous Solution. Synthesis, Structure, and Reactivity of the Functionalized Heteropolytungstates, [XW11O39RhCH2COOH]5,6- (X = P, Si)
Xinyi Wei; Michael H. Dickman; Michael T. Pope; Journal of the American Chemical Society 120 (1998) 10254–10255; doi:10.1021/ja980993p

data_4116841
_publ_contact_author
;
      Prof. Michael T. Pope
      Department of Chemistry
      Georgetown University
      Washington, D.C. 20057
      USA
;
_publ_contact_author_email       POPE@GUVAX.ACC.GEORGETOWN.EDU
_publ_contact_author_fax         '202 687 6209'
_publ_contact_author_phone       '202 687 6253'
_publ_section_title
;
 Rhodium-Carbon Bond Formation in Aqueous Solution. Synthesis, Structure,
 and Reactivity of the Functionalized Heteropolytungstates,
 [XW11O39RhCH2COOH]5,6- (X = P, Si)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10254
_journal_page_last               10255
_journal_paper_doi               10.1021/ja980993p
_journal_volume                  120
_journal_year                    1998
_chemical_compound_source        synthesized
_chemical_formula_sum            'C2 Cs6 O44 Rh Si W11'
_chemical_formula_weight         3678.83
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 94.4080(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.2577(2)
_cell_length_b                   22.9293(5)
_cell_length_c                   17.6274(4)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.56
_cell_measurement_theta_min      1.46
_cell_volume                     4536.72(16)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_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 CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0836
_diffrn_reflns_av_sigmaI/netI    0.0566
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            45857
_diffrn_reflns_theta_max         30.56
_diffrn_reflns_theta_min         1.46
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    32.996
_exptl_absorpt_correction_T_max  0.0227
_exptl_absorpt_correction_T_min  0.0013
_exptl_absorpt_correction_type   Blessing
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    5.386
_exptl_crystal_description       plate
_exptl_crystal_F_000             6268
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         3.804
_refine_diff_density_min         -2.777
_refine_diff_density_rms         0.554
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.113
_refine_ls_goodness_of_fit_obs   1.159
_refine_ls_matrix_type           full
_refine_ls_number_parameters     588
_refine_ls_number_reflns         13478
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.113
_refine_ls_restrained_S_obs      1.159
_refine_ls_R_factor_all          0.0820
_refine_ls_R_factor_obs          0.0667
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0748P)^2^+160.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1708
_refine_ls_wR_factor_obs         0.1612
_reflns_number_observed          11126
_reflns_number_total             13478
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja980993p.cif
_cod_data_source_block           siw
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0748P)^2^+160.0000P] 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^)+(0.0748P)^2^+160.0000P] 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        4536.7(2)
_cod_database_code               4116841