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_4347713
_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_compound_source        'see text'
_chemical_formula_moiety
'C23 H30 N10 Ru, 2(F6 P), C4 H10 O, 0.5(C2 H3 N)'
_chemical_formula_sum            'C28 H41.5 F12 N10.5 O P2 Ru'
_chemical_formula_weight         932.21
_space_group_IT_number           114
_space_group_name_Hall           'P -4 2n'
_space_group_name_H-M_alt        'P -4 21 c'
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      114
_symmetry_space_group_name_Hall  'P -4 2n'
_symmetry_space_group_name_H-M   'P -4 21 c'
_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                   19.5906(6)
_cell_length_b                   19.5906(6)
_cell_length_c                   20.6319(7)
_cell_measurement_reflns_used    9978
_cell_measurement_temperature    123
_cell_measurement_theta_max      26.4405
_cell_measurement_theta_min      2.3016
_cell_volume                     7918.4(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 1.000
_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  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1656
_diffrn_reflns_av_sigmaI/netI    0.0666
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            154307
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         1.43
_exptl_absorpt_coefficient_mu    0.572
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5480
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker, 2008b'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.564
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             3784
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.24
_platon_squeeze_details
;
The unit cell contains 4 disordered molecules of acetonitrile on a 
special position which were treated as a diffuse contribution to 
the overall scattering without specific atom positions by 
SQUEEZE/PLATON.
;
_refine_diff_density_max         0.447
_refine_diff_density_min         -0.819
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   0.62(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     783
_refine_ls_number_reflns         7260
_refine_ls_number_restraints     1481
_refine_ls_restrained_S_all      0.948
_refine_ls_R_factor_all          0.0998
_refine_ls_R_factor_gt           0.0500
_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^)+(0.0473P)^2^+8.7268P] WHERE P=(FO^2^+2FC^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1014
_refine_ls_wR_factor_ref         0.1211
_reflns_number_gt                4755
_reflns_number_total             7260
_reflns_threshold_expression     i>2\s(i)
_cod_data_source_file            ic6b00509_si_002.cif
_cod_data_source_block           compound_2
_cod_original_cell_volume        7918.4(6)
_cod_original_formula_sum        'C28 H41.50 F12 N10.50 O P2 Ru'
_cod_database_code               4347713