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_7038102
_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         'C35 H51.5 P2 Ru S2'
_chemical_formula_sum            'C35 H51.5 P2 Ru S2'
_chemical_formula_weight         699.44
_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                 96.735(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.3215(10)
_cell_length_b                   17.7887(19)
_cell_length_c                   22.489(3)
_cell_measurement_reflns_used    6410
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.69
_cell_measurement_theta_min      2.34
_cell_volume                     3306.0(7)
_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      150.04
_diffrn_measured_fraction_theta_full 0.9910
_diffrn_measured_fraction_theta_max 0.9910
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0731
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            52981
_diffrn_reflns_theta_full        27.5598
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         1.46
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.721
_exptl_absorpt_correction_T_max  0.7422
_exptl_absorpt_correction_T_min  0.6648
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1006 before and 0.0832 after correction.
The Ratio of minimum to maximum transmission is 0.8957.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_density_diffrn    1.4052
_exptl_crystal_description       Blocks
_exptl_crystal_F_000             1467.2182
_refine_diff_density_max         0.7220
_refine_diff_density_min         -1.3698
_refine_diff_density_rms         0.1364
_refine_ls_d_res_high            0.7681
_refine_ls_d_res_low             13.9144
_refine_ls_goodness_of_fit_ref   1.0292
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    98
_refine_ls_number_parameters     381
_refine_ls_number_reflns         7577
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.0289
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0354
_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^)+(0.0372P)^2^+2.8800P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0808
_refine_ls_wR_factor_ref         0.0885
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              9
_reflns_limit_h_min              -10
_reflns_limit_k_max              23
_reflns_limit_k_min              0
_reflns_limit_l_max              28
_reflns_limit_l_min              -8
_reflns_number_gt                5988
_reflns_number_total             7577
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c5dt04481b2.cif
_cod_data_source_block           AMM043_0m
_cod_database_code               7038102
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 C11-C12 = C12-C13 = C11-C12a = C12a-C13
 1.54 with sigma of 0.01
3. Others
 Fixed Sof: H11(0.5) H13c(0.5) H13d(0.5) H13a(0.5) H13b(0.5) C15a(0.5)
 H15c(0.5) H15d(0.5) H16c(0.5) H16d(0.5) H16a(0.5) H16b(0.5) C15(0.5) H15a(0.5)
 H15b(0.5) C12(0.5) H12b(0.5) H12c(0.5) H12a(0.5) C14(0.5) H14a(0.5) H14b(0.5)
 C14a(0.5) H14c(0.5) H14d(0.5) H11(0.5) H12a(0.5) H12b(0.5) H11(0.5) H13c(0.5)
 H13d(0.5) H13a(0.5) H13b(0.5) H12a(0.5) H12b(0.5) C2aa(0.25) C12(0.5)
 C12a(0.5) H11(0.5) H13a(0.5) H13b(0.5) H13c(0.5) H13d(0.5) H12a(0.5) H12b(0.5)
 H12c(0.5) H12d(0.5)
4.a Ternary CH refined with riding coordinates:
 C17(H17), C23(H23), C11(H11)
4.b Secondary CH2 refined with riding coordinates:
 C1(H1a,H1b), C2(H2a,H2b), C9(H9a,H9b), C10(H10a,H10b), C18(H18a,H18b),
 C19(H19a,H19b), C20(H20a,H20b), C21(H21a,H21b), C22(H22a,H22b), C24(H24a,H24b),
  C25(H25a,H25b), C26(H26a,H26b), C27(H27a,H27b), C28(H28a,H28b), C15a(H15c,
 H15d), C16(H16c,H16d), C16(H16a,H16b), C15(H15a,H15b), C14(H14a,H14b),
 C14a(H14c,H14d), C13(H13a,H13b), C13(H13c,H13d), C12(H12a,H12b), C12a(H12c,
 H12d)
4.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C31(H31), C32(H32), C33(H33),
 C34(H34), C35(H35)
;
_olex2_submission_special_instructions 'No special instructions were received'