Alkene-Chelated Ruthenium Alkylidenes: A Missing Link to New Catalysts
Gupta, Saswata; Sabbasani, Venkata R.; Su, Siyuan; Wink, Donald J.; Lee, Daesung; ACS Catalysis 11 (2021) 1977–1987; doi:10.1021/acscatal.0c04972

data_4518442
_publ_section_title
;
 Alkene-Chelated Ruthenium Alkylidenes: A Missing Link to New Catalysts
;
_journal_issue                   4
_journal_name_full               'ACS Catalysis'
_journal_page_first              1977
_journal_page_last               1987
_journal_paper_doi               10.1021/acscatal.0c04972
_journal_volume                  11
_journal_year                    2021
_chemical_formula_sum            'C38 H46 Cl2 N2 Ru'
_chemical_formula_weight         702.74
_chemical_name_common            vs_Ru_db_coord2
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'APEX2 v2014.5-0'
_cell_angle_alpha                90
_cell_angle_beta                 93.972(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.9816(10)
_cell_length_b                   10.5576(7)
_cell_length_c                   13.8098(12)
_cell_measurement_reflns_used    6176
_cell_measurement_temperature    200.(2)
_cell_measurement_theta_max      23.5446
_cell_measurement_theta_min      2.1740
_cell_volume                     1742.7(2)
_computing_cell_refinement       'SAINT v7.68A (Bruker AXS Inc.)'
_computing_data_reduction        'SAINT v7.68A (Bruker AXS Inc.)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200.(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART X2S benchtop diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'doubly curved silicon crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0595
_diffrn_reflns_av_unetI/netI     0.0612
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17704
_diffrn_reflns_theta_full        25.07
_diffrn_reflns_theta_max         25.07
_diffrn_reflns_theta_min         1.48
_diffrn_source                   'XOS X-beam microfocus source'
_exptl_absorpt_coefficient_mu    0.631
_exptl_absorpt_correction_T_max  0.91
_exptl_absorpt_correction_T_min  0.64
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             732
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.160
_refine_diff_density_max         0.453
_refine_diff_density_min         -0.595
_refine_ls_abs_structure_details
;
Flack x determined using 2175 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.599
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     396
_refine_ls_number_reflns         5926
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.599
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0358
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1455P)^2^+1.1547P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0995
_refine_ls_wR_factor_ref         0.1149
_reflns_number_gt                5252
_reflns_number_total             5926
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs0c04972_si_002.cif
_cod_data_source_block           Compound_10a
_cod_depositor_comments
'Adding full bibliography for 4518430--4518444.cif.'
_cod_database_code               4518442
_publ_contact_phone              312-413-7383
_publ_contact_fax                312-996-0431
_publ_contact_email              dwink@uic.edu