Use of the monocationic fragment [Ru(η5-C5H5)(MeCN)3]+ as an ionic coupling reagent in the synthesis of mixed-metal phosphine clusters †
Buntem, Radchada; Gallagher, John F.; Lewis, Jack; Raithby, Paul R.; Rennie, Moira-Ann; Shields, Gregory P.; Journal of the Chemical Society, Dalton Transactions  (2000) 4297–; doi:10.1039/b006746f

data_7010191
_publ_section_title
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 Use of the monocationic fragment [Ru(\h5-C5H5)(MeCN)3]+ as an ionic
 coupling reagent in the synthesis of mixed-metal phosphine
 clusters&#x200A;&#x2020;
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_journal_issue                   23
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4297
_journal_paper_doi               10.1039/b006746f
_journal_year                    2000
_chemical_formula_sum            'C34 H21 O11 Os3 P Ru'
_chemical_formula_weight         1308.15
_chemical_name_systematic
; 
 ? 
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_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 114.06(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.878(4)
_cell_length_b                   22.669(17)
_cell_length_c                   9.415(4)
_cell_measurement_temperature    290(2)
_cell_volume                     1730.2(18)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      290(2)
_diffrn_measurement_device       'Stoe-Siemens four-circle diffractometer'
_diffrn_measurement_method       'omega/theta 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  0.1280
_diffrn_reflns_av_sigmaI/netI    0.1260
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            5552
_diffrn_reflns_theta_max         23.99
_diffrn_reflns_theta_min         3.59
_diffrn_standards_interval_time  '60 minutes'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    11.514
_exptl_absorpt_correction_T_max  0.526
_exptl_absorpt_correction_T_min  0.401
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            'Dark Red/Purple'
_exptl_crystal_density_diffrn    2.511
_exptl_crystal_description       Block
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.23
_refine_diff_density_max         2.987
_refine_diff_density_min         -1.329
_refine_diff_density_rms         0.236
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_coef       0.0021(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.175
_refine_ls_goodness_of_fit_obs   1.178
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         2787
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.169
_refine_ls_restrained_S_obs      1.168
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_obs          0.0462
_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^)+(0.0191P)^2^+8.7521P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1080
_refine_ls_wR_factor_obs         0.1055
_reflns_number_observed          2670
_reflns_number_total             2788
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b006746f.txt
_cod_data_source_block           ldb07
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0191P)^2^+8.7521P] 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^)+(0.0191P)^2^+8.7521P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_cell_volume        1730.2(17)
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               7010191