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_4346140
_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            'C34.5 H47 Cl2 N2 P2 Ru'
_chemical_formula_weight         723.65
_chemical_name_common            'in manuscript 3b'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                85.5090(12)
_cell_angle_beta                 82.1460(12)
_cell_angle_gamma                78.1590(12)
_cell_formula_units_Z            4
_cell_length_a                   11.6983(5)
_cell_length_b                   17.3524(8)
_cell_length_c                   17.5483(8)
_cell_measurement_reflns_used    5888
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      24.90
_cell_measurement_theta_min      2.26
_cell_volume                     3449.0(3)
_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 0.978
_diffrn_measured_fraction_theta_max 0.998
_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  0.0651
_diffrn_reflns_av_unetI/netI     0.0952
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            33075
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.055
_diffrn_reflns_theta_min         1.173
_diffrn_source                   'ImuS microsource'
_exptl_absorpt_coefficient_mu    0.728
_exptl_absorpt_correction_T_max  0.9628
_exptl_absorpt_correction_T_min  0.8613
_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
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_exptl_crystal_description       plate
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.504
_refine_diff_density_min         -0.475
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     832
_refine_ls_number_reflns         12204
_refine_ls_number_restraints     1009
_refine_ls_restrained_S_all      0.964
_refine_ls_R_factor_all          0.0906
_refine_ls_R_factor_gt           0.0453
_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^)+(0.0329P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_reflns_number_gt                7929
_reflns_number_total             12204
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00513_si_002.cif
_cod_data_source_block           chb16
_cod_original_formula_sum        'C34.50 H47 Cl2 N2 P2 Ru'
_cod_database_code               4346140
_shelx_estimated_absorpt_t_min   0.918
_shelx_estimated_absorpt_t_max   0.951
_shelxl_version_number           2013-4
_shelx_res_checksum              55817
_shelx_hkl_checksum              84596