Five-Coordinate Hydrido−Ruthenium(II) Complexes Featuring N-Heterocyclic Silylene and Carbene Ligands
Cade, Ian A.; Hill, Anthony F.; Kämpfe, Alexander; Wagler, Jörg; Organometallics 29 (2010) 4012–; doi:10.1021/om100146m

data_4065810
_publ_section_title
;
 Five-Coordinate Hydrido&#x2212;Ruthenium(II) Complexes Featuring
 N-Heterocyclic Silylene and Carbene Ligands
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              4012
_journal_paper_doi               10.1021/om100146m
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C46 H87 Cl N2 P2 Ru Si, 2.5(C6 H6)'
_chemical_formula_sum            'C61 H102 Cl N2 P2 Ru Si'
_chemical_formula_weight         1090.05
_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                94.7153(7)
_cell_angle_beta                 100.6340(7)
_cell_angle_gamma                101.9604(7)
_cell_formula_units_Z            2
_cell_length_a                   10.5987(1)
_cell_length_b                   14.3344(1)
_cell_length_c                   20.7699(3)
_cell_measurement_reflns_used    69700
_cell_measurement_temperature    200
_cell_measurement_theta_max      30
_cell_measurement_theta_min      2.6
_cell_volume                     3010.07(6)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows v. 2.01'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      200
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.058
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            82935
_diffrn_reflns_theta_full        30.037
_diffrn_reflns_theta_max         30.037
_diffrn_reflns_theta_min         2.632
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.415
_exptl_absorpt_correction_T_max  0.952
_exptl_absorpt_correction_T_min  0.882
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1174
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.82
_refine_diff_density_min         -1.06
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.8641
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     617
_refine_ls_number_reflns         17552
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0364
_refine_ls_shift/su_max          0.001328
_refine_ls_structure_factor_coef Fsqd
_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: 
 36.2 56.6 28.6 7.41 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1799
_refine_ls_wR_factor_gt          0.1258
_refine_ls_wR_factor_ref         0.1799
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              20
_reflns_limit_k_min              -20
_reflns_limit_l_max              29
_reflns_limit_l_min              0
_reflns_number_gt                12071
_reflns_number_total             17588
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.89
_oxford_diffrn_Wilson_scale      16.36
_oxford_refine_ls_r_factor_ref   0.0617
_oxford_refine_ls_scale          0.2471(2)
_oxford_reflns_number_all        17552
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            om100146m_si_001.cif
_cod_data_source_block           1
_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_original_formula_sum        'C61 H102 Cl1 N2 P2 Ru1 Si1'
_cod_database_code               4065810