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_7038106
_publ_section_title
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 Ru Alkylidene Compounds Bearing Tridentate, Dianionic Ligands: Lewis Acid
 Activation and Olefin Metathesis
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_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C5DT04481B
_journal_year                    2016
_chemical_formula_moiety         'C31 H50 B Cl2 N O P Ru S2, B Cl4'
_chemical_formula_sum            'C31 H50 B2 Cl6 N O P Ru S2'
_chemical_formula_weight         883.28
_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                 100.467(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5984(5)
_cell_length_b                   13.8097(7)
_cell_length_c                   27.2535(15)
_cell_measurement_temperature    149
_cell_volume                     3922.5(3)
_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 0.9966
_diffrn_measured_fraction_theta_max 0.9966
_diffrn_measurement_device_type  Bruker_Apex_II
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0778
_diffrn_reflns_av_unetI/netI     0.0872
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            36241
_diffrn_reflns_theta_full        27.8990
_diffrn_reflns_theta_max         27.90
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    0.983
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6612
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0685 before and 0.0581 after correction.
The Ratio of minimum to maximum transmission is 0.8868.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.4956
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1816.4030
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.3645
_refine_diff_density_min         -1.3009
_refine_diff_density_rms         0.2197
_refine_ls_d_res_high            0.7595
_refine_ls_d_res_low             12.2758
_refine_ls_goodness_of_fit_ref   1.0116
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    77
_refine_ls_number_parameters     410
_refine_ls_number_reflns         9330
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0116
_refine_ls_R_factor_all          0.0893
_refine_ls_R_factor_gt           0.0453
_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^)+(0.0370P)^2^+1.6937P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0866
_refine_ls_wR_factor_ref         0.1029
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -13
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              35
_reflns_limit_l_min              -11
_reflns_number_gt                6104
_reflns_number_total             9330
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c5dt04481b2.cif
_cod_data_source_block           AMM034_0m
_cod_original_cell_volume        3922.5(4)
_cod_database_code               7038106
_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:
 C13(H13), C19(H19), C25(H25)
2.b Secondary CH2 refined with riding coordinates:
 C8(H8a,H8b), C9(H9a,H9b), C10(H10a,H10b), C11(H11a,H11b), C14(H14a,H14b),
 C15(H15a,H15b), C16(H16a,H16b), C17(H17a,H17b), C18(H18a,H18b), C20(H20a,H20b),
  C21(H21a,H21b), C22(H22a,H22b), C23(H23a,H23b), C24(H24a,H24b), C26(H26a,
 H26b), C27(H27a,H27b), C28(H28a,H28b), C29(H29a,H29b), C30(H30a,H30b)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7)
2.d Idealised Me refined as rotating group:
 C31(H31a,H31b,H31c)
;
_olex2_submission_special_instructions 'No special instructions were received'