Controlling Coordination Geometries: Ru-Carbene Complexes with Tetra-NHC Ligands.
Hollering, Manuela; Weiss, Daniel T.; Bitzer, Mario J.; Jandl, Christian; Kühn, Fritz E; Inorganic chemistry 55 (2016) 6010–6017; doi:10.1021/acs.inorgchem.6b00509

data_4347715
_publ_section_title
;
 Controlling Coordination Geometries: Ru-Carbene Complexes with Tetra-NHC
 Ligands.
;
_journal_issue                   12
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6010
_journal_page_last               6017
_journal_paper_doi               10.1021/acs.inorgchem.6b00509
_journal_volume                  55
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C23 H38 N8 P2 Ru, 2(F6 P), 2(C2 H3 N)'
_chemical_formula_sum            'C27 H44 F12 N10 P4 Ru'
_chemical_formula_weight         961.67
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      43
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.1959(6)
_cell_length_b                   26.4637(8)
_cell_length_c                   14.6327(4)
_cell_measurement_reflns_used    9955
_cell_measurement_temperature    123
_cell_measurement_theta_max      30.5131
_cell_measurement_theta_min      2.5373
_cell_volume                     7820.6(4)
_computing_cell_refinement       'SAINT (Bruker, 2012)'
_computing_data_collection       'APEX II Control Software (Bruker, 2013)'
_computing_data_reduction        'SAINT (Bruker, 2012)'
_computing_molecular_graphics    'PLATON (Spek, 2011)'
_computing_publication_material  'PLATON (Spek, 2011), enCIFer (Allen, 2004)'
_computing_structure_refinement
'SHELXL2014 (Sheldrick, 2014), SHELXLE (Huebschle, 2011)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      123
_diffrn_detector                 ' CCD plate '
_diffrn_detector_area_resol_mean 16
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       ' \k-geometry diffractometer '
_diffrn_measurement_device_type  ' Bruker APEX-II CCD '
_diffrn_measurement_method       ' phi- and omega-rotation '
_diffrn_radiation_monochromator  'MONTEL optic'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'rotating anode FR591'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_av_sigmaI/netI    0.0173
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            77305
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    0.658
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5287
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker, 2008b'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             3904
_exptl_crystal_size_max          0.563
_exptl_crystal_size_mid          0.259
_exptl_crystal_size_min          0.258
_refine_diff_density_max         0.492
_refine_diff_density_min         -0.353
_refine_diff_density_rms         0.117
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   0.012(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         4863
_refine_ls_number_restraints     286
_refine_ls_restrained_S_all      1.235
_refine_ls_R_factor_all          0.0225
_refine_ls_R_factor_gt           0.0219
_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^)+(0.0380P)^2^+6.7590P] WHERE P=(FO^2^+2FC^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0598
_refine_ls_wR_factor_ref         0.0604
_reflns_number_gt                4767
_reflns_number_total             4863
_reflns_threshold_expression     i>2\s(i)
_cod_data_source_file            ic6b00509_si_002.cif
_cod_data_source_block           compound_1c
_cod_database_code               4347715