Tetrasilacyclobutadiene and Cyclobutadiene Tricarbonylruthenium Complexes: [η4-(tBu2MeSi)4Si4]Ru(CO)3and [η4-(Me3Si)4C4]Ru(CO)3
Takanashi, Kazunori; Lee, Vladimir Ya.; Sekiguchi, Akira; Organometallics 28 (2009) 1248–; doi:10.1021/om801128h

data_4083446
_publ_section_title
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 Tetrasilacyclobutadiene and Cyclobutadiene Tricarbonylruthenium
 Complexes: [\h4-(tBu2MeSi)4Si4]Ru(CO)3and [\h4-(Me3Si)4C4]Ru(CO)3
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_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              1248
_journal_paper_doi               10.1021/om801128h
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C39 H84 O3 Ru Si8'
_chemical_formula_weight         926.85
_chemical_name_systematic
; 
(tBu2MeSi)4Si4Ru(CO)3 
;
_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                93.585(2)
_cell_angle_beta                 90.930(3)
_cell_angle_gamma                92.055(2)
_cell_formula_units_Z            4
_cell_length_a                   15.1370(7)
_cell_length_b                   17.5450(7)
_cell_length_c                   19.5900(5)
_cell_measurement_reflns_used    51040
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      27.99
_cell_measurement_theta_min      2.06
_cell_volume                     5188.3(3)
_computing_cell_refinement       'HKL scalepack'
_computing_data_collection       'MacScience Xpress'
_computing_data_reduction        Denzo
_computing_molecular_graphics    ORTEP
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      120(1)
_diffrn_measured_fraction_theta_full 0.914
_diffrn_measured_fraction_theta_max 0.914
_diffrn_measurement_device       'MacScience DIP2030 Image plate'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.049
_diffrn_reflns_av_sigmaI/netI    0.0668
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            51040
_diffrn_reflns_theta_full        27.99
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    0.518
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_diffrn    1.187
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             1992
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.700
_refine_diff_density_min         -0.992
_refine_diff_density_rms         0.092
_refine_ls_extinction_coef       0.0048(2)
_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_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     920
_refine_ls_number_reflns         22861
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0695
_refine_ls_R_factor_gt           0.0470
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0675P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1166
_refine_ls_wR_factor_ref         0.1255
_reflns_number_gt                16958
_reflns_number_total             22861
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om801128h_si_002.cif
_cod_data_source_block           shelxl
_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 
;
_cod_original_sg_symbol_H-M      'P -1          '
_cod_database_code               4083446