Bulky N-Phosphino-Functionalized N-Heterocyclic Carbene Ligands: Synthesis, Ruthenium Coordination Chemistry, and Ruthenium Alkylidene Complexes for Olefin Metathesis.
Brown, Christopher C.; Rominger, Frank; Limbach, Michael; Hofmann, Peter; Inorganic chemistry 54 (2015) 10126–10140; doi:10.1021/acs.inorgchem.5b00513

data_4346141
_publ_section_title
;
 Bulky N-Phosphino-Functionalized N-Heterocyclic Carbene Ligands:
 Synthesis, Ruthenium Coordination Chemistry, and Ruthenium Alkylidene
 Complexes for Olefin Metathesis.
;
_journal_issue                   21
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10126
_journal_page_last               10140
_journal_paper_doi               10.1021/acs.inorgchem.5b00513
_journal_volume                  54
_journal_year                    2015
_chemical_formula_sum            'C34 H46 Cl4 N2 P2 Ru'
_chemical_formula_weight         787.54
_chemical_name_common            'in manuscript 3c'
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 91.141(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5570(10)
_cell_length_b                   17.4081(17)
_cell_length_c                   19.9446(18)
_cell_measurement_reflns_used    3449
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      24.71
_cell_measurement_theta_min      2.20
_cell_volume                     3664.6(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.950
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II Quazar'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0712
_diffrn_reflns_av_unetI/netI     0.1656
_diffrn_reflns_Laue_measured_fraction_full 0.950
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            21833
_diffrn_reflns_point_group_measured_fraction_full 0.933
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.807
_diffrn_reflns_theta_min         1.021
_diffrn_source                   'ImuS microsource'
_exptl_absorpt_coefficient_mu    0.833
_exptl_absorpt_correction_T_max  0.9621
_exptl_absorpt_correction_T_min  0.7526
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Sheldrick, G. M. (2008). <i>SADABS</i>. University of G\"ottingen, Germany.
;
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_description       plate
_exptl_crystal_F_000             1624
_exptl_crystal_size_max          0.090
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.060
_refine_diff_density_max         1.136
_refine_diff_density_min         -1.127
_refine_diff_density_rms         0.135
_refine_ls_abs_structure_details
; 
 Flack x determined using 2628 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   0.13(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     775
_refine_ls_number_reflns         12376
_refine_ls_number_restraints     721
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.1421
_refine_ls_R_factor_gt           0.0765
_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^)+(0.0247P)^2^+6.2140P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1059
_refine_ls_wR_factor_ref         0.1268
_reflns_Friedel_coverage         0.898
_reflns_Friedel_fraction_full    0.916
_reflns_Friedel_fraction_max     0.961
_reflns_number_gt                8056
_reflns_number_total             12376
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00513_si_002.cif
_cod_data_source_block           chb15
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4346141
_shelx_estimated_absorpt_t_min   0.929
_shelx_estimated_absorpt_t_max   0.952
_shelxl_version_number           2013-4
_shelx_res_checksum              94712
_shelx_hkl_checksum              5742