Synthesis of Diruthenium μ-η4-α-Diimine Complex via Dehydrogenative Coupling of Cyclic Amines and Its Role in Dehydrogenative Oxidation of Pyrrolidine
Takao, Toshihiro; Shimogawa, Ryuichi; Fujita, Ryosuke; Egawa, Shu; Dalton Transactions  (2023) –; doi:10.1039/D3DT03187J

data_7714277
_publ_section_title
;
 Synthesis of Diruthenium \m-\h4-\a-Diimine Complex via Dehydrogenative
 Coupling of Cyclic Amines and Its Role in Dehydrogenative Oxidation of
 Pyrrolidine
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT03187J
_journal_year                    2023
_chemical_formula_sum            'C44 H74 N2 Ru2'
_chemical_formula_weight         833.19
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2023-09-21 deposited with the CCDC.	2023-10-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.6250(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7555(3)
_cell_length_b                   35.2527(11)
_cell_length_c                   11.1031(4)
_cell_measurement_reflns_used    66445
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      27.478
_cell_measurement_theta_min      2.999
_cell_volume                     4172.6(2)
_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      143(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_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  0.0911
_diffrn_reflns_av_unetI/netI     0.0559
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            65797
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         27.478
_diffrn_reflns_theta_min         2.999
_diffrn_source                   'Rigaku Rotating Anode Ultrax18'
_exptl_absorpt_coefficient_mu    0.755
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7578
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSCOR (T. Higashi, 2001)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.108
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.061
_refine_diff_density_max         1.538
_refine_diff_density_min         -1.258
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         9526
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0657
_refine_ls_R_factor_gt           0.0457
_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^)+(0.0350P)^2^+7.2962P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0950
_refine_ls_wR_factor_ref         0.1041
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7430
_reflns_number_total             9526
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03187j5.cif
_cod_data_source_block           5d
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Empirical' was
changed to 'empirical' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/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 8170 2020-07-09 18:12:32Z antanas 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7714277
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.923
_shelx_estimated_absorpt_t_max   0.955
_shelx_res_checksum              11856