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_7038103
_publ_section_title
;
 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         'C32 H40 N2 O3 Ru'
_chemical_formula_sum            'C32 H40 N2 O3 Ru'
_chemical_formula_weight         601.75
_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                 95.679(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.6299(6)
_cell_length_b                   14.408(1)
_cell_length_c                   21.2995(14)
_cell_measurement_temperature    149
_cell_volume                     2940.7(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      149.69
_diffrn_measured_fraction_theta_full 0.9955
_diffrn_measured_fraction_theta_max 0.9952
_diffrn_measurement_device_type  Bruker_Apex_II
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            33894
_diffrn_reflns_theta_full        30.2799
_diffrn_reflns_theta_max         30.28
_diffrn_reflns_theta_min         1.71
_exptl_absorpt_coefficient_mu    0.567
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6890
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0542 before and 0.0420 after correction.
The Ratio of minimum to maximum transmission is 0.9236.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_density_diffrn    1.3591
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1251.5034
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.2743
_refine_diff_density_min         -1.3293
_refine_diff_density_rms         0.1129
_refine_ls_d_res_high            0.7048
_refine_ls_d_res_low             11.9156
_refine_ls_goodness_of_fit_ref   1.0395
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    57
_refine_ls_number_parameters     360
_refine_ls_number_reflns         8753
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0395
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0380
_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^)+(0.0181P)^2^+6.1128P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0796
_refine_ls_wR_factor_ref         0.0869
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              11
_reflns_limit_h_min              -13
_reflns_limit_k_max              20
_reflns_limit_k_min              0
_reflns_limit_l_max              30
_reflns_limit_l_min              -11
_reflns_number_gt                7308
_reflns_number_total             8753
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c5dt04481b2.cif
_cod_data_source_block           AMM044_0m
_cod_database_code               7038103
_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
3.a Secondary CH2 refined with riding coordinates:
 C3(H3a,H3b), C2(H2a,H2b), C23(H23a,H23b), C22(H22a,H22b), C24(H24a,H24b)
3.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C15(H15), C8(H8), C6(H6), C28(H28), C29(H29), C30(H30), C31(H31),
 C32(H32)
3.c Idealised Me refined as rotating group:
 C21(H21a,H21b,H21c), C20(H20a,H20b,H20c), C19(H19a,H19b,H19c), C11(H11a,H11b,
 H11c), C10(H10a,H10b,H10c), C12(H12a,H12b,H12c)
;
_olex2_submission_special_instructions 'No special instructions were received'