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_4088582
_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 H62 Cl O P Ru S, C5 H12'
_chemical_formula_sum            'C57 H74 Cl O P Ru S'
_chemical_formula_weight         974.71
_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                 97.968(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.419(3)
_cell_length_b                   15.046(3)
_cell_length_c                   27.038(6)
_cell_measurement_reflns_used    9968
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      24.86
_cell_measurement_theta_min      2.49
_cell_volume                     5003.4(19)
_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 0.997
_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  0.1360
_diffrn_reflns_av_unetI/netI     0.0928
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            52714
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.359
_diffrn_reflns_theta_min         1.724
_diffrn_source                   'rotating anode'
_exptl_absorpt_coefficient_mu    0.479
_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            'dark purple'
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_description       'irregular prism'
_exptl_crystal_F_000             2064
_exptl_crystal_size_max          0.344
_exptl_crystal_size_mid          0.226
_exptl_crystal_size_min          0.108
_exptl_transmission_factor_max   1.000
_exptl_transmission_factor_min   0.7720
_refine_diff_density_max         2.386
_refine_diff_density_min         -1.334
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.163
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     563
_refine_ls_number_reflns         9135
_refine_ls_number_restraints     504
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.1388
_refine_ls_R_factor_gt           0.0975
_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^)+(0.0001P)^2^+60.6058P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1851
_refine_ls_wR_factor_ref         0.2004
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6492
_reflns_number_total             9135
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00214_si_003.cif
_cod_data_source_block           Compound4
_cod_original_cell_volume        5003.5(17)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4088582
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              48272
_shelx_hkl_checksum              58020