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_4088583
_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         'C48 H51 O2 P Ru S, C H2 Cl2'
_chemical_formula_sum            'C49 H53 Cl2 O2 P Ru S'
_chemical_formula_weight         908.91
_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-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 105.4360(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8196(5)
_cell_length_b                   17.0380(6)
_cell_length_c                   20.3621(7)
_cell_measurement_reflns_used    9886
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      30.02
_cell_measurement_theta_min      2.39
_cell_volume                     4287.1(3)
_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  0.0771
_diffrn_reflns_av_unetI/netI     0.0531
_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       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            71691
_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         30.060
_diffrn_reflns_theta_min         2.036
_diffrn_source                   'rotating anode'
_exptl_absorpt_coefficient_mu    0.616
_exptl_absorpt_correction_type   numerical
_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
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_description       'irregular prism'
_exptl_crystal_F_000             1888
_exptl_crystal_size_max          0.177
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.040
_exptl_transmission_factor_max   1.000
_exptl_transmission_factor_min   0.7097
_refine_diff_density_max         2.970
_refine_diff_density_min         -0.794
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     513
_refine_ls_number_reflns         12539
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_gt           0.0405
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0513P)^2^+1.6780P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0995
_refine_ls_wR_factor_ref         0.1059
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10038
_reflns_number_total             12539
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00214_si_005.cif
_cod_data_source_block           Compound8b
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4088583
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.899
_shelx_estimated_absorpt_t_max   0.976
_shelx_res_checksum              50995
_shelx_hkl_checksum              57642