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_4518444
_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_moiety         'C48 H57 Cl2 N3 O3 Ru S'
_chemical_formula_sum            'C48 H57 Cl2 N3 O3 Ru S'
_chemical_formula_weight         927.99
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-08-07
_audit_creation_method
;
Olex2 1.2
(compiled 2017.07.20 svn.r3457 for OlexSys, GUI svn.r5370)
;
_audit_update_record
;
2020-07-23 # Formatted by publCIF

;
_cell_angle_alpha                90
_cell_angle_beta                 96.636(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.6853(18)
_cell_length_b                   12.842(2)
_cell_length_c                   32.754(5)
_cell_measurement_reflns_used    9772
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      24.92
_cell_measurement_theta_min      2.26
_cell_volume                     5300.0(14)
_computing_cell_refinement       'APEX2 (Bruker, 2011); SAINT (Bruker, 2009)'
_computing_data_collection       'GIS (Bruker)'
_computing_data_reduction
'SAINT (Bruker, 2009); XPREP (Sheldrick, 2008)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0577
_diffrn_reflns_av_unetI/netI     0.0394
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            54576
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.068
_diffrn_reflns_theta_max         25.068
_diffrn_reflns_theta_min         2.020
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.473
_exptl_absorpt_correction_T_max  0.8671
_exptl_absorpt_correction_T_min  0.5343
_exptl_absorpt_process_details
'Sheldrick, G. M. (2008) SADABS. University of G\"ottingen, Germany.'
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.163
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       amygdaloidal
_exptl_crystal_F_000             1936
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.31
_refine_diff_density_max         0.586
_refine_diff_density_min         -1.086
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         9368
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0626
_refine_ls_R_factor_gt           0.0543
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0525P)^2^+9.5609P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1286
_refine_ls_wR_factor_ref         0.1330
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8058
_reflns_number_total             9368
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs0c04972_si_006.cif
_cod_data_source_block           Compound_10q
_cod_depositor_comments
'Adding full bibliography for 4518430--4518444.cif.'
_cod_original_cell_volume        5299.8(13)
_cod_database_code               4518444
_publ_contact_phone              312-413-7383
_publ_contact_fax                312-996-0431
_publ_contact_email              dwink@uic.edu
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.867
_shelx_estimated_absorpt_t_min   0.812
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C4(H4A,H4B), C14(H14A,H14B), C15(H15A,H15B), C29(H29A,H29B),
 C30(H30A,H30B)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C9(H9), C10(H10), C12(H12), C13(H13), C20(H20), C21(H21), C23(H23),
 C24(H24), C25(H25), C26(H26), C27(H27), C34(H34), C36(H36), C43(H43), C45(H45)
2.c X=CH2 refined with riding coordinates:
 C6(H6A,H6B)
2.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C33(H33A,H33B,H33C), C38(H38A,H38B,
 H38C), C39(H39A,H39B,H39C), C42(H42A,H42B,H42C), C47(H47A,H47B,H47C), C48(H48A,
 H48B,H48C), C49(H49A,H49B,H49C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_publcif_funding_html
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;