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_4346138
_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            'C15 H28 F3 N2 O3 P S'
_chemical_formula_weight         404.42
_chemical_name_common            'in manuscript 1b'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.3820(11)
_cell_length_b                   10.5135(7)
_cell_length_c                   11.8675(8)
_cell_measurement_reflns_used    3586
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      23.32
_cell_measurement_theta_min      2.49
_cell_volume                     2044.0(2)
_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 1.000
_diffrn_measured_fraction_theta_max 0.996
_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  0.0529
_diffrn_reflns_av_unetI/netI     0.0611
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13547
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.722
_diffrn_reflns_theta_min         2.119
_diffrn_source                   'ImuS microsource'
_exptl_absorpt_coefficient_mu    0.279
_exptl_absorpt_correction_T_max  0.9582
_exptl_absorpt_correction_T_min  0.8273
_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            colourless
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.592
_refine_diff_density_min         -0.563
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details
; 
 Flack x determined using 1146 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   -0.01(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3885
_refine_ls_number_restraints     189
_refine_ls_restrained_S_all      1.148
_refine_ls_R_factor_all          0.0822
_refine_ls_R_factor_gt           0.0654
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0188P)^2^+5.4741P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1339
_refine_ls_wR_factor_ref         0.1414
_reflns_Friedel_coverage         0.746
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                3172
_reflns_number_total             3885
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00513_si_002.cif
_cod_data_source_block           chb14
_cod_database_code               4346138
_shelx_estimated_absorpt_t_min   0.952
_shelx_estimated_absorpt_t_max   0.986
_shelxl_version_number           2013-4
_shelx_res_checksum              7870
_shelx_hkl_checksum              4966