Phosphine-Based Z-Selective Ruthenium Olefin Metathesis Catalysts
Smit, Wietse; Koudriavtsev, Vitali; Occhipinti, Giovanni; Törnroos, Karl W.; Jensen, Vidar R.; Organometallics 35 (2016) 1825–; doi:10.1021/acs.organomet.6b00214

data_4088581
_publ_section_title
;
 Phosphine-Based Z-Selective Ruthenium Olefin Metathesis Catalysts
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              1825
_journal_paper_doi               10.1021/acs.organomet.6b00214
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C52 H55 O4 P Ru S2, C H2 Cl2'
_chemical_formula_sum            'C53 H57 Cl2 O4 P Ru S2'
_chemical_formula_weight         1025.04
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 94.9320(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0441(10)
_cell_length_b                   23.8002(18)
_cell_length_c                   15.4295(12)
_cell_measurement_reflns_used    9753
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      30.96
_cell_measurement_theta_min      2.30
_cell_volume                     4772.4(6)
_computing_cell_refinement       'SAINT. Ver. 8.34A. Bruker-AXS, 2014'
_computing_data_collection       'APEX2. Ver. 2014.11-0. Bruker-AXS, 2014'
_computing_data_reduction        'SAINT. Ver. 8.34A. Bruker-AXS, 2014'
_computing_structure_refinement
;
SHELXL-2014/7. Sheldrick G.M., Acta Cryst. (2015). C71, 3-8.
;
_computing_structure_solution
;
SHELXT. Sheldrick G.M., Acta Cryst. (2015). A71, 3-8.
;
_diffrn_ambient_temperature      103(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            84499
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.000
_diffrn_reflns_theta_min         1.711
_diffrn_source                   'rotating anode'
_exptl_absorpt_coefficient_mu    0.607
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS. Ver. 2014/3 
Krause, L., Herbst-Irmer, R., Sheldrick, G. M. & Stalke, D. (2015). 
J. Appl. Crystallogr. 48.
;
_exptl_crystal_colour            purple-brown
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_description       'irregular prism'
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.11
_exptl_transmission_factor_max   0.7462
_exptl_transmission_factor_min   0.6000
_refine_diff_density_max         1.366
_refine_diff_density_min         -0.940
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     570
_refine_ls_number_reflns         15193
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0411
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0488P)^2^+6.5861P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1030
_refine_ls_wR_factor_ref         0.1086
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13180
_reflns_number_total             15193
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00214_si_004.cif
_cod_data_source_block           Compound6
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4088581
_shelxl_version_number           2014-2
_shelx_res_checksum              66683
_shelx_hkl_checksum              61202