A Stable Silylene in a Reactive Environment: Synthesis, Reactivity, and Silicon Extrusion Chemistry of a Coordinatively Unsaturated Ruthenium Silylene Complex Containing Chloride and η3-P‒C‒P Ligands
Amoroso, Dino; Haaf, Michael; Yap, Glenn P. A.; West, Robert; Fogg, Deryn E.; Organometallics 21 (2002) 534–540; doi:10.1021/om0101801

data_4084050
_publ_section_title
; 
 A Stable Silylene in a Reactive Environment: Synthesis, Reactivity,
 and Silicon Extrusion Chemistry of a Coordinatively Unsaturated
 Ruthenium Silylene Complex Containing Chloride and \h3-P--C--P Ligands
;
_journal_coden_ASTM              ORGND7
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              534
_journal_page_last               540
_journal_paper_doi               10.1021/om0101801
_journal_volume                  21
_journal_year                    2002
_chemical_formula_sum            'C62 H109 Cl3 N2 P4 Ru2'
_chemical_formula_weight         1314.88
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                89.7230(10)
_cell_angle_beta                 86.8370(10)
_cell_angle_gamma                66.5080(10)
_cell_formula_units_Z            2
_cell_length_a                   11.6220(9)
_cell_length_b                   13.5699(10)
_cell_length_c                   22.7781(17)
_cell_measurement_reflns_used    'reflections from 60 data frames'
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      1.47
_cell_volume                     3289.0(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.876
_diffrn_measured_fraction_theta_max 0.876
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0404
_diffrn_reflns_av_sigmaI/netI    0.0943
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_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            25795
_diffrn_reflns_theta_full        28.71
_diffrn_reflns_theta_max         28.71
_diffrn_reflns_theta_min         1.64
_diffrn_standards_decay_%        <1
_diffrn_standards_number         '50 standard frames at start and end'
_exptl_absorpt_coefficient_mu    0.716
_exptl_absorpt_correction_T_max  0.928076
_exptl_absorpt_correction_T_min  0.828149
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing,R., Acta Cryst. (1995) A51 33-38.'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1388
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.965
_refine_diff_density_min         -0.696
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     658
_refine_ls_number_reflns         14910
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0971
_refine_ls_R_factor_gt           0.0487
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0964
_refine_ls_wR_factor_ref         0.1059
_reflns_number_gt                9029
_reflns_number_total             14910
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0101801.cif
_cod_data_source_block           df021
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Updated bibliographic information.

 Antanas Vaitkus,
 2019-10-02
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4084050