Solid-State Structure and Solution Reactivity of [(Ph3P)4Ru(H)2] and Related Ru(II) Complexes Used in Catalysis: A Reinvestigation
Samouei, Hamidreza; Miloserdov, Fedor M.; Escudero-Adán, Eduardo C.; Grushin, Vladimir V.; Organometallics 33 (2014) 7279–; doi:10.1021/om5010572

data_4084871
_publ_section_title
;
 Solid-State Structure and Solution Reactivity of [(Ph3P)4Ru(H)2] and
 Related Ru(II) Complexes Used in Catalysis: A Reinvestigation
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              7279
_journal_paper_doi               10.1021/om5010572
_journal_volume                  33
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_sum            'C62 H65 O2 P3 Ru'
_chemical_formula_weight         1036.12
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
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_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
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_cell_angle_gamma                90
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_cell_length_b                   21.30(2)
_cell_length_c                   24.96(3)
_cell_measurement_reflns_used    21
_cell_measurement_temperature    100(2)
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_cell_measurement_theta_min      4.46
_cell_volume                     5080(8)
_computing_cell_refinement       'Bruker APEX2 v2011.4-0'
_computing_data_collection       'Bruker APEX2 v2011.4-0'
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_computing_molecular_graphics    'Bruker SHELXTL'
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_computing_structure_solution    Sir2011
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 512
_diffrn_detector_type            '4K CCD area detector APEX II'
_diffrn_measured_fraction_theta_full 0.778
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'APEX DUO Kappa 4-axis goniometer'
_diffrn_measurement_method
;
 Fullsphere data collection, phi and omega scans
;
_diffrn_measurement_specimen_support 'magnetic support with MicroMount'
_diffrn_radiation_monochromator  'Quazar MX Multilayer Optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.1171
_diffrn_reflns_Laue_measured_fraction_full 0.778
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_point_group_measured_fraction_full 0.434
_diffrn_reflns_point_group_measured_fraction_max 0.560
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         23.046
_diffrn_reflns_theta_min         1.257
_diffrn_source                   'Microfocus source E025 IuS'
_diffrn_source_current           0.6
_diffrn_source_power             50
_diffrn_source_size              '0.2 mm x 0.2 mm fine focus'
_diffrn_source_type              'Bruker APEX DUO'
_exptl_absorpt_coefficient_mu    0.448
_exptl_absorpt_correction_T_max  0.9955
_exptl_absorpt_correction_T_min  0.9566
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
 TWINABS Version 2008/0 Bruker-Nonius
 Blessing, Acta Cryst. (1995) A51 33-38
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_description       needle
_exptl_crystal_F_000             2168
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.01
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_refine_diff_density_min         -1.159
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_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.38(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
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_refine_ls_number_restraints     390
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.1006
_refine_ls_R_factor_gt           0.0719
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.1092P)^2^+2.7123P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1653
_refine_ls_wR_factor_ref         0.1817
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3114
_reflns_number_total             3994
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5010572_si_001.cif
_cod_data_source_block           mo_HRS507-04
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/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 2935 2014-11-11 08:27:57Z andrius 

 Adding full bibliography for 4084867--4084875.cif.
;
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               4084871
_shelx_estimated_absorpt_t_min   0.957
_shelx_estimated_absorpt_t_max   0.996
_shelxl_version_number           2012-9
_shelx_res_checksum              7907
_shelx_hkl_checksum              15886