Synthesis and Dynamic Properties of a Triruthenium Complex Containing μ3-η2(∥)-Ethyne and μ3-Methylidyne Ligands: Equilibrium of an Ethyne‒Hydrido Complex with a Nonclassical μ3-Vinyl Complex
Tahara, Atsushi; Kajigaya, Mana; Takao, Toshiro; Suzuki, Hiroharu; Organometallics 32 (2013) 260–; doi:10.1021/om301064y

data_4079931
_publ_section_title
;
 Synthesis and Dynamic Properties of a Triruthenium Complex Containing
 \m3-\h2(&#x2225;)-Ethyne and \m3-Methylidyne Ligands: Equilibrium of an
 Ethyne--Hydrido Complex with a Nonclassical \m3-Vinyl Complex
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              260
_journal_paper_doi               10.1021/om301064y
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C44 H63 N Ru3'
_chemical_formula_weight         909.16
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
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_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.8700(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.0349(4)
_cell_length_b                   10.8512(3)
_cell_length_c                   20.3620(4)
_cell_measurement_reflns_used    37262
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.00
_cell_volume                     3955.41(16)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'SHELXS-97 (Sheldrick, 1990)'
_computing_molecular_graphics    'ORTEX (P.McArdle, 1995)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SHELXS-97
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku Rotating Anode ultraX18'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
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_diffrn_reflns_av_sigmaI/netI    0.0607
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_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
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_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    1.161
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6346
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1864
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_exptl_crystal_size_mid          0.172
_exptl_crystal_size_min          0.115
_refine_diff_density_max         1.835
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_refine_ls_extinction_method     none
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_refine_ls_number_parameters     541
_refine_ls_number_reflns         9046
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_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0306
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0055P)^2^+3.9161P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_refine_ls_wR_factor_ref         0.0736
_reflns_number_gt                8322
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_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om301064y_si_002.cif
_cod_data_source_block           6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        3955.41(17)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4079931