Diruthenium Complexes Having a Partially Hydrogenated Bipyridine Ligand: Plausible Mechanism for the Dehydrogenative Coupling of Pyridines at a Diruthenium Site
Takao, Toshihiro; Kawashima, Takashi; Nagae, Ryo; Kanda, Hideyuki; Watanabe, Wataru; Faraday Discussions  (2019) –; doi:10.1039/C9FD00029A

data_1550951
_publ_section_title
;
 Diruthenium Complexes Having a Partially Hydrogenated Bipyridine Ligand:
 Plausible Mechanism for the Dehydrogenative Coupling of Pyridines at a
 Diruthenium Site
;
_journal_name_full               'Faraday Discussions'
_journal_paper_doi               10.1039/C9FD00029A
_journal_year                    2019
_chemical_formula_sum            'C32 H46 N2 Ru2'
_chemical_formula_weight         660.85
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2019-03-05 deposited with the CCDC.    2019-04-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.3836(8)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.7520(6)
_cell_length_b                   8.49780(19)
_cell_length_c                   34.8959(7)
_cell_measurement_reflns_used    33032
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      29.985
_cell_measurement_theta_min      3.050
_cell_volume                     5742.0(2)
_computing_cell_refinement       'RAPID AUTO (Rigaku, 2015)'
_computing_data_collection       'RAPID AUTO (Rigaku, 2015)'
_computing_data_reduction        'RAPID AUTO (Rigaku, 2015)'
_computing_molecular_graphics    'ORTEX (P.McArdle, 1995)'
_computing_publication_material  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.981
_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  0.0290
_diffrn_reflns_av_unetI/netI     0.0255
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            31904
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         29.985
_diffrn_reflns_theta_min         3.050
_diffrn_source                   'Rigaku Rotating Anode Ultrax18'
_exptl_absorpt_coefficient_mu    1.075
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8708
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             2720
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.837
_refine_diff_density_min         -0.631
_refine_diff_density_rms         0.076
_refine_ls_extinction_coef       0.00050(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         8193
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0268
_refine_ls_R_factor_gt           0.0224
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0157P)^2^+9.2811P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0486
_refine_ls_wR_factor_ref         0.0504
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7393
_reflns_number_total             8193
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9fd00029a2.cif
_cod_data_source_block           4a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Empirical' changed to
'empirical' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

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

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_database_code               1550951
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.882
_shelx_estimated_absorpt_t_max   0.938
_shelx_res_checksum              73571