Ru Alkylidene Compounds Bearing Tridentate, Dianionic Ligands: Lewis Acid Activation and Olefin Metathesis
McKinty, Adam; Stephan, Douglas W.; Dalton Trans.  (2016) –; doi:10.1039/C5DT04481B

data_7038104
_publ_section_title
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 Ru Alkylidene Compounds Bearing Tridentate, Dianionic Ligands: Lewis Acid
 Activation and Olefin Metathesis
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C5DT04481B
_journal_year                    2016
_chemical_formula_moiety         'C29 H47 B Cl3 O P Ru S2'
_chemical_formula_sum            'C29 H47 B Cl3 O P Ru S2'
_chemical_formula_weight         725.05
_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'
_audit_creation_date             2015-07-15
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-07-15 deposited with the CCDC.
2016-01-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.048(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.7135(6)
_cell_length_b                   10.0800(3)
_cell_length_c                   19.4358(7)
_cell_measurement_temperature    149
_cell_volume                     3280.29(19)
_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      150.0
_diffrn_measured_fraction_theta_full 0.9992
_diffrn_measured_fraction_theta_max 0.9992
_diffrn_measurement_device_type  Bruker_Apex_II
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_unetI/netI     0.0406
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            50915
_diffrn_reflns_theta_full        33.5969
_diffrn_reflns_theta_max         33.60
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    0.921
_exptl_absorpt_correction_T_max  0.7466
_exptl_absorpt_correction_T_min  0.6670
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0518 before and 0.0467 after correction.
The Ratio of minimum to maximum transmission is 0.8934.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.4680
_exptl_crystal_description       Blocks
_exptl_crystal_F_000             1502.5812
_refine_diff_density_max         1.0755
_refine_diff_density_min         -0.7087
_refine_diff_density_rms         0.1325
_refine_ls_d_res_high            0.6422
_refine_ls_d_res_low             10.7510
_refine_ls_goodness_of_fit_ref   1.0170
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    75
_refine_ls_number_parameters     342
_refine_ls_number_reflns         12965
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0170
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0310
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0296P)^2^+0.6630P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0650
_refine_ls_wR_factor_ref         0.0725
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              16
_reflns_limit_h_min              -27
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              30
_reflns_limit_l_min              -16
_reflns_number_gt                10021
_reflns_number_total             12965
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c5dt04481b2.cif
_cod_data_source_block           AMM_Stephan_0m
_cod_database_code               7038104
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C5(H5), C11(H11), C17(H17)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1a,H1b), C2(H2a,H2b), C3(H3a,H3b), C4(H4a,H4b), C6(H6a,H6b), C7(H7a,H7b),
 C8(H8a,H8b), C9(H9a,H9b), C10(H10a,H10b), C12(H12a,H12b), C13(H13a,H13b),
 C14(H14a,H14b), C15(H15a,H15b), C16(H16a,H16b), C18(H18a,H18b), C19(H19a,H19b),
  C20(H20a,H20b), C21(H21a,H21b), C22(H22a,H22b)
2.c Aromatic/amide H refined with riding coordinates:
 C23(H23), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29)
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_olex2_submission_special_instructions 'No special instructions were received'