Photoinduced Reactions of Diruthenium Tetrahydride Complexes: Carbon‒Hydrogen Bond Cleavage of Tetrahydrofuran Leading to Bridging Cyclic Fischer-Type Carbene Complexes
Shimogawa, Ryuichi; Konishi, Gen-ichi; Takao, Toshiro; Suzuki, Hiroharu; Organometallics 35 (2016) 1446–; doi:10.1021/acs.organomet.6b00070

data_4088424
_publ_section_title
;
 Photoinduced Reactions of Diruthenium Tetrahydride Complexes:
 Carbon--Hydrogen Bond Cleavage of Tetrahydrofuran Leading to Bridging
 Cyclic Fischer-Type Carbene Complexes
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              1446
_journal_paper_doi               10.1021/acs.organomet.6b00070
_journal_volume                  35
_journal_year                    2016
_chemical_formula_sum            'C38 H66 O Ru2'
_chemical_formula_weight         741.04
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 103.059(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.2806(6)
_cell_length_b                   11.8219(7)
_cell_length_c                   15.4868(10)
_cell_measurement_reflns_used    18302
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.459
_cell_measurement_theta_min      3.189
_cell_volume                     1833.53(19)
_computing_cell_refinement       'RAPID AUTO (Rigaku, 2006)'
_computing_data_collection       'RAPID AUTO (Rigaku, 2006)'
_computing_data_reduction        'RAPID AUTO (Rigaku, 2006)'
_computing_molecular_graphics    'ORTEX (P.McArdle, 1995)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 10
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_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_av_unetI/netI     0.0439
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
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_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
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_diffrn_reflns_limit_l_min       -20
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_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.978
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_diffrn_reflns_theta_max         27.459
_diffrn_reflns_theta_min         3.189
_diffrn_source                   'Rigaku Rotating Anode Ultrax18'
_exptl_absorpt_coefficient_mu    0.850
_exptl_absorpt_correction_T_max  0.8787
_exptl_absorpt_correction_T_min  0.8124
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (T. Higashi, 1999)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             780
_exptl_crystal_size_max          0.321
_exptl_crystal_size_mid          0.183
_exptl_crystal_size_min          0.173
_refine_diff_density_max         0.462
_refine_diff_density_min         -0.470
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details
;
 Flack x determined using 3803 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.016(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     465
_refine_ls_number_reflns         8224
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0283
_refine_ls_R_factor_gt           0.0275
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0389P)^2^+0.5791P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0703
_refine_ls_wR_factor_ref         0.0711
_reflns_Friedel_coverage         0.958
_reflns_Friedel_fraction_full    0.978
_reflns_Friedel_fraction_max     0.958
_reflns_number_gt                8063
_reflns_number_total             8224
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00070_si_002.cif
_cod_data_source_block           tbucpthf_a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Numerical' was
changed to 'numerical' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

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

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      'P n'
_cod_database_code               4088424
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.772
_shelx_estimated_absorpt_t_max   0.867
_shelx_res_checksum              18845
_shelx_hkl_checksum              3326