Disentangling Ligand Effects on Metathesis Catalyst Activity: Experimental and Computational Studies of Ruthenium-Aminophosphine Complexes.
Chu, Crystal K.; Lin, Tzu-Pin; Shao, Huiling; Liberman-Martin, Allegra L; Liu, Peng; Grubbs, Robert H.; Journal of the American Chemical Society 140 (2018) 5634–5643; doi:10.1021/jacs.8b02324

data_4132191
_publ_section_title
;
 Disentangling Ligand Effects on Metathesis Catalyst Activity:
 Experimental and Computational Studies of Ruthenium-Aminophosphine
 Complexes.
;
_journal_issue                   16
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5634
_journal_page_last               5643
_journal_paper_doi               10.1021/jacs.8b02324
_journal_volume                  140
_journal_year                    2018
_chemical_formula_sum            'C50 H76 Cl2 N4 O1.5 P Ru'
_chemical_formula_weight         960.08
_chemical_name_common            CyPpip2
_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-97
_cell_angle_alpha                90
_cell_angle_beta                 102.711(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.582(4)
_cell_length_b                   14.694(4)
_cell_length_c                   26.929(9)
_cell_measurement_reflns_used    9872
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      60.270
_cell_measurement_theta_min      4.877
_cell_volume                     4857(3)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.922
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0561
_diffrn_reflns_av_unetI/netI     0.0580
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.922
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            109331
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.922
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.312
_diffrn_reflns_theta_min         2.080
_exptl_absorpt_coefficient_mu    0.507
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9533
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_description       block
_exptl_crystal_F_000             2036
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.020
_refine_diff_density_max         2.255
_refine_diff_density_min         -1.253
_refine_diff_density_rms         0.194
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     538
_refine_ls_number_reflns         14689
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.1013
_refine_ls_R_factor_gt           0.0645
_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^)+(0.0672P)^2^+17.5230P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1465
_refine_ls_wR_factor_ref         0.1643
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10910
_reflns_number_total             14689
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b02324_si_003.cif
_cod_data_source_block           mm
_cod_depositor_comments
;

2021-04-11
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C100 H152 Cl4 N8 O3 P2 Ru2 Si0'
_cod_original_formula_weight         1920.17
_cod_original_formula_units_Z            2
_cod_original_cell_volume        4856(3)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4132191
_shelx_estimated_absorpt_t_min   0.928
_shelx_estimated_absorpt_t_max   0.990
_shelxl_version_number           2013-2
_shelx_res_checksum              42954