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_7038105
_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         'C32 H40 B Cl3 N2 Ru S3, 0.5(C Cl2)'
_chemical_formula_sum            'C32.5 H40 B Cl4 N2 Ru S3'
_chemical_formula_weight         808.59
_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'
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 124.733(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.498(3)
_cell_length_b                   10.7156(10)
_cell_length_c                   23.057(2)
_cell_measurement_temperature    149
_cell_volume                     7004.7(11)
_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 0.9965
_diffrn_measured_fraction_theta_max 0.9965
_diffrn_measurement_device_type  Bruker_Apex_II
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_av_unetI/netI     0.0479
_diffrn_reflns_limit_h_max       51
_diffrn_reflns_limit_h_min       -49
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            45387
_diffrn_reflns_theta_full        32.0467
_diffrn_reflns_theta_max         32.05
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    0.959
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.6476
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0623 before and 0.0507 after correction.
The Ratio of minimum to maximum transmission is 0.8676.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.5333
_exptl_crystal_description       blocks
_exptl_crystal_F_000             3310.5309
_exptl_crystal_size_max          0.319
_exptl_crystal_size_mid          0.245
_exptl_crystal_size_min          0.201
_refine_diff_density_max         1.0118
_refine_diff_density_min         -1.0537
_refine_diff_density_rms         0.1479
_refine_ls_d_res_high            0.6697
_refine_ls_d_res_low             10.0235
_refine_ls_goodness_of_fit_ref   1.0236
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    60
_refine_ls_number_parameters     415
_refine_ls_number_reflns         12148
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.0235
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0345
_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^)+(0.0343P)^2^+7.1427P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0764
_refine_ls_wR_factor_ref         0.0846
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              42
_reflns_limit_h_min              -51
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              34
_reflns_limit_l_min              0
_reflns_number_gt                9426
_reflns_number_total             12148
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c5dt04481b2.cif
_cod_data_source_block           AMM015_0m
_cod_original_cell_volume        7004.7(12)
_cod_database_code               7038105
_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. Restrained distances
 c35-Cl4 = c35-Cl5
 1.7 with sigma of 0.01
3. Others
 Fixed Sof: Cl4(0.5) Cl5(0.5) c35(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1a,H1b), C2(H2a,H2b), C3(H3a,H3b), C4(H4a,H4b), C16(H16a,H16b), C17(H17a,
 H17b)
4.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C11(H11), C22(H22), C25(H25), C30(H30), C31(H31), C32(H32), C33(H33),
 C34(H34)
4.c Idealised Me refined as rotating group:
 C13(H13a,H13b,H13c), C14(H14a,H14b,H14c), C15(H15a,H15b,H15c), C21(H21a,H21b,
 H21c), C24(H24a,H24b,H24c), C27(H27a,H27b,H27c)
;
_olex2_submission_special_instructions 'No special instructions were received'