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_1554276
_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         'C42 H49 Cl2 N3 O3 Ru S'
_chemical_formula_sum            'C42 H49 Cl2 N3 O3 Ru S'
_chemical_formula_weight         847.91
_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'
_symmetry_Int_Tables_number      14
_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                 107.451(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3662(8)
_cell_length_b                   19.3514(12)
_cell_length_c                   18.2778(11)
_cell_measurement_reflns_used    9912
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      24.2015
_cell_measurement_theta_min      2.2413
_cell_volume                     4510.0(5)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_diffrn_ambient_temperature      300.15
_diffrn_measured_fraction_theta_full 0.9989
_diffrn_measured_fraction_theta_max 0.9989
_diffrn_measurement_device_type  'Bruker SMART X2S'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            92652
_diffrn_reflns_theta_full        26.3700
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.10
_exptl_absorpt_coefficient_mu    0.550
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.2487
_exptl_crystal_description       plate
_exptl_crystal_F_000             1757.3062
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.6288
_refine_diff_density_min         -0.3541
_refine_diff_density_rms         0.0936
_refine_ls_d_res_high            0.8001
_refine_ls_d_res_low             9.6757
_refine_ls_goodness_of_fit_ref   1.0356
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    77
_refine_ls_number_parameters     479
_refine_ls_number_reflns         9202
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0356
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0425
_refine_ls_shift/su_max          0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0703P)^2^+2.5649P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1139
_refine_ls_wR_factor_ref         0.1226
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              11
_reflns_limit_h_min              -16
_reflns_limit_k_max              24
_reflns_limit_k_min              0
_reflns_limit_l_max              22
_reflns_limit_l_min              -10
_reflns_number_gt                7403
_reflns_number_total             9202
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c8qo00160j3.cif
_cod_data_source_block           venkata_p21n_a
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_database_code               1554276
_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
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4.a Ternary CH refined with riding coordinates:
 C00Y(H00Y)
4.b Secondary CH2 refined with riding coordinates:
 C00J(H00a,H00b), C00V(H00c,H00d), C013(H01g,H01h)
4.c Aromatic/amide H refined with riding coordinates:
 C01C(H01w), C01A(H01u), C01F(H01z), C015(H015), C00K(H00K), C00N(H00N),
 C00S(H00S), C00Q(H00Q), C01B(H01v), C01G(H01), C01I(H0aa), C01D(H01x),
 C00W(H00W), C00X(H00X)
4.d Idealised Me refined as rotating group:
 C00Z(H00e,H00f,H00g), C010(H01a,H01b,H01c), C012(H01d,H01e,H01f), C014(H01i,
 H01j,H01k), C017(H01l,H01m,H01n), C018(H01o,H01p,H01q), C019(H01r,H01s,H01t),
 C01E(H01y,H,Ha), C01J(H1aa,Hb,Hc)
4.e Idealised tetrahedral OH refined as rotating group:
 O10(H10)
;
_olex2_submission_special_instructions 'No special instructions were received'