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_1554277
_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         'C33 H46 Cl2 N2 O Ru'
_chemical_formula_sum            'C33 H46 Cl2 N2 O Ru'
_chemical_formula_weight         658.69
_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   mixed
_atom_sites_solution_primary     dual
_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                 104.49(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.573(10)
_cell_length_b                   14.783(10)
_cell_length_c                   16.116(10)
_cell_measurement_reflns_used    6795
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      2.1690
_cell_measurement_theta_min      26.4010
_cell_volume                     3361(4)
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      300.15
_diffrn_measured_fraction_theta_full 0.940
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'Bruker SMART X2S'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1175
_diffrn_reflns_av_unetI/netI     0.0939
_diffrn_reflns_Laue_measured_fraction_full 0.940
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            44849
_diffrn_reflns_point_group_measured_fraction_full 0.940
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         1.443
_exptl_absorpt_coefficient_mu    0.652
_exptl_absorpt_correction_T_max  0.88
_exptl_absorpt_correction_T_min  0.60
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.55
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.600
_refine_diff_density_min         -2.456
_refine_diff_density_rms         0.287
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.281
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         7324
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.281
_refine_ls_R_factor_all          0.1839
_refine_ls_R_factor_gt           0.1163
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2790
_refine_ls_wR_factor_ref         0.3651
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4378
_reflns_number_total             7324
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8qo00160j2.cif
_cod_data_source_block           ru_bu_a
_cod_database_code               1554277
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.881
_shelx_estimated_absorpt_t_min   0.696
_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, All O(H) groups
2. Restrained distances
 O004-H004
 0.85 with sigma of 0.01
 C10-H004
 1.920127 with sigma of 0.02
 Ru01-H004
 2.932527 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C10(H10)
3.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C8(H8A,H8B), C15(H15A,H15B), C2(H2A,H2B), C14(H14A,H14B), C3(H3A,
 H3B)
3.c Aromatic/amide H refined with riding coordinates:
 C29(H29), C7(H7), C18(H18), C20(H20), C27(H27)
3.d Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C12(H12A,H12B,H12C), C24(H24A,H24B,H24C), C22(H22A,H22B,
 H22C), C11(H11A,H11B,H11C), C23(H23A,H23B,H23C), C32(H32A,H32B,H32C), C33(H33A,
 H33B,H33C), C1(H1A,H1B,H1C)
;
_olex2_submission_special_instructions 'No special instructions were received'