Synthesis and Reactions of Five-Coordinate Mono- and Binuclear Thiocarbonyl−Alkenyl and Thioacyl Complexes of Ruthenium(II)
Cowley, Andrew R.; Hector, Andrew L.; Hill, Anthony F.; White, Andrew J. P.; Williams, David J.; Wilton-Ely, James D. E. T.; Organometallics 26 (2007) 6114–; doi:10.1021/om700518m

data_4073663
_publ_section_title
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 Synthesis and Reactions of Five-Coordinate Mono- and Binuclear
 Thiocarbonyl&#x2212;Alkenyl and Thioacyl Complexes of Ruthenium(II)
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_journal_issue                   25
_journal_name_full               Organometallics
_journal_page_first              6114
_journal_paper_doi               10.1021/om700518m
_journal_volume                  26
_journal_year                    2007
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C53 H41 Cl P2 Ru S, C H2 Cl2'
_chemical_formula_sum            'C54 H43 Cl3 P2 Ru S'
_chemical_formula_weight         993.38
_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_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                75.0004(7)
_cell_angle_beta                 78.8495(7)
_cell_angle_gamma                63.7609(10)
_cell_formula_units_Z            2
_cell_length_a                   12.1475(2)
_cell_length_b                   12.2581(2)
_cell_length_c                   18.0528(3)
_cell_measurement_reflns_used    38750
_cell_measurement_temperature    150
_cell_measurement_theta_max      28
_cell_measurement_theta_min      5
_cell_volume                     2319.31(7)
_computing_cell_refinement
; 
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) 
;
_computing_data_collection
; 
KappaCCD software 'Collect' (Nonius, 2000) 
;
_computing_data_reduction
; 
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) 
;
_computing_publication_material
; 
CRYSTALS (Watkin et al, 2001) 
;
_computing_structure_refinement
; 
CRYSTALS (Watkin et al, 2001) 
;
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1992)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
; 
Nonius KappaCCD 
;
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_reflns_av_R_equivalents  0.057
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            38750
_diffrn_reflns_theta_full        27.442
_diffrn_reflns_theta_max         27.442
_diffrn_reflns_theta_min         5.135
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.662
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.89
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_description       block
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_exptl_crystal_thermal_history
; 
The material was crystallised at ambient temperature. A suitable crystal 
was cooled rapidly to 150K for single-crystal X-ray diffraction analysis. 
;
_refine_diff_density_max         1.81
_refine_diff_density_min         -1.35
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0960
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         6508
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0810
_refine_ls_R_factor_gt           0.0444
_refine_ls_shift/su_max          0.001209
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.543 0.305 0.269 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0845
_refine_ls_wR_factor_gt          0.0508
_refine_ls_wR_factor_ref         0.0508
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              15
_reflns_limit_k_min              -15
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                6508
_reflns_number_total             10505
_reflns_threshold_expression     I>3.00u(I)
_oxford_refine_ls_scale          0.1792(3)
_cod_data_source_file            om700518m-file002.cif
_cod_data_source_block           Compound_4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4073663