A general approach for the formation of oxygen-chelated ruthenium alkylidene complexes relying on the Thorpe‒Ingold effect
Sabbasani, Venkata R.; Gupta, Saswata; Young Yun, Sang; Lee, Daesung; Organic Chemistry Frontiers 5 (2018) 1532–; doi:10.1039/C8QO00160J

data_1554278
_publ_section_title
;
 A general approach for the formation of oxygen-chelated ruthenium
 alkylidene complexes relying on the Thorpe--Ingold effect
;
_journal_issue                   9
_journal_name_full               'Organic Chemistry Frontiers'
_journal_page_first              1532
_journal_paper_doi               10.1039/C8QO00160J
_journal_volume                  5
_journal_year                    2018
_chemical_formula_moiety         'C36 H44 Cl2 N2 O Ru'
_chemical_formula_sum            'C36 H44 Cl2 N2 O Ru'
_chemical_formula_weight         692.70
_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'
_atom_sites_solution_hydrogens   mixed
_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
;
2017-11-09 deposited with the CCDC.
2018-03-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.100(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   26.317(4)
_cell_length_b                   17.570(2)
_cell_length_c                   17.431(2)
_cell_measurement_reflns_used    9881
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      24.99
_cell_measurement_theta_min      2.46
_cell_volume                     7569.0(17)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      200.15
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0492
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            39117
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.094
_diffrn_reflns_theta_max         25.094
_diffrn_reflns_theta_min         1.422
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.582
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.216
_exptl_crystal_description       prism
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.941
_refine_diff_density_min         -0.365
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         6671
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0417
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0609P)^2^+22.6192P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1117
_refine_ls_wR_factor_ref         0.1240
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5571
_reflns_number_total             6671
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8qo00160j2.cif
_cod_data_source_block           scan_0m_c2_c
_cod_original_cell_volume        7569.1(17)
_cod_database_code               1554278
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.892
_shelx_estimated_absorpt_t_min   0.759
_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 Ternary CH refined with riding coordinates:
 C31(H31)
2.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B), C34(H34A,H34B), C35(H35A,H35B)
2.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C7(H7), C17(H17), C19(H19), C25(H25), C26(H26), C27(H27), C28(H28),
 C29(H29), C36(H36)
2.d Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C16(H16A,H16B,H16C),
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C33(H33A,H33B,H33C), C37(H37A,H37B,
 H37C)
;
_olex2_submission_special_instructions 'No special instructions were received'