New Structural Motifs Resulting from Internal Constraints in Chelating Bis(NHC) Ligands: A Dinuclear Ruthenium(II) Complex Featuring an η2-Arene Binding Mode and a Remarkable New Tetrameric Silver(I) Halide Form
Simpson, Peter V.; Brown, David H.; Skelton, Brian W.; White, Allan H.; Baker, Murray V.; Organometallics 34 (2015) 2508–; doi:10.1021/om5012165

data_4085593
_publ_section_title
;
 New Structural Motifs Resulting from Internal Constraints in Chelating
 Bis(NHC) Ligands: A Dinuclear Ruthenium(II) Complex Featuring an
 \h2-Arene Binding Mode and a Remarkable New Tetrameric Silver(I) Halide
 Form
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2508
_journal_paper_doi               10.1021/om5012165
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C40 H56 N4 O4, 2(Cl), H2 O'
_chemical_formula_sum            'C40 H58 Cl2 N4 O5'
_chemical_formula_weight         745.8
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-06-05T10:08:49-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 98.312(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   31.1544(15)
_cell_length_b                   15.0002(8)
_cell_length_c                   17.3313(8)
_cell_measurement_reflns_used    3596
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      67.0569
_cell_measurement_theta_min      2.8676
_cell_volume                     8014.2(7)
_computing_cell_refinement
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
        (compiled Nov  6 2009,16:24:50)
;
_computing_data_collection
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
        (compiled Nov  6 2009,16:24:50)
;
_computing_data_reduction
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
        (compiled Nov  6 2009,16:24:50)
;
_computing_molecular_graphics    'Diamond (Brandenburg, K., (1999)'
_computing_publication_material  'WinGX Farrugia, L. J. (1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4738
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Oxford Diffraction Gemini diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0197208363
_diffrn_orient_matrix_UB_12      0.0812422511
_diffrn_orient_matrix_UB_13      -0.0362846643
_diffrn_orient_matrix_UB_21      -0.0375188042
_diffrn_orient_matrix_UB_22      0.0584689934
_diffrn_orient_matrix_UB_23      0.0194813516
_diffrn_orient_matrix_UB_31      0.0262607879
_diffrn_orient_matrix_UB_32      0.0226768746
_diffrn_orient_matrix_UB_33      0.0797708847
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0614
_diffrn_reflns_av_unetI/netI     0.0661
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
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_diffrn_reflns_limit_l_min       -15
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_diffrn_reflns_theta_full        67.23
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_exptl_absorpt_coefficient_mu    1.829
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.79778
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
      CrysAlis RED, Oxford Diffraction Ltd.,
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.

;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             3200
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.424
_refine_diff_density_min         -0.269
_refine_diff_density_rms         0.05
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.97
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         7098
_refine_ls_number_restraints     116
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.1171
_refine_ls_R_factor_gt           0.061
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0972P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1545
_refine_ls_wR_factor_ref         0.1821
_reflns_number_gt                3933
_reflns_number_total             7098
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om5012165_si_002.cif
_cod_data_source_block           ps295b
_cod_depositor_comments
'Adding full bibliography for 4085592--4085594.cif.'
_cod_original_sg_symbol_Hall     '-c 2yc'
_cod_database_code               4085593