From Simple Ligands to Complex Structures: Structural Diversity of Silver(I) Complexes Bearing Tetradentate (alkylenebimpy) NHC Ligands
Wagner, Thomas; Pöthig, Alexander; Augenstein, Hannah M. S.; Schmidt, Tobias D.; Kaposi, Marlene; Herdtweck, Eberhard; Brütting, Wolfgang; Herrmann, Wolfgang A.; Kühn, Fritz E.; Organometallics  (2015) 150410094812000–; doi:10.1021/om5013067

data_4085809
_publ_section_title
;
 From Simple Ligands to Complex Structures: Structural Diversity of
 Silver(I) Complexes Bearing Tetradentate (alkylenebimpy) NHC Ligands
;
_journal_name_full               Organometallics
_journal_page_first              150410094812000
_journal_paper_doi               10.1021/om5013067
_journal_year                    2015
_chemical_formula_moiety         'C66 H72 Ag4 N18, 4(F6 P), 2(C2 H3 N)'
_chemical_formula_sum            'C70 H78 Ag4 F24 N20 P4'
_chemical_formula_weight         2210.88
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                79.455(2)
_cell_angle_beta                 66.860(1)
_cell_angle_gamma                70.499(2)
_cell_formula_units_Z            1
_cell_length_a                   12.6618(4)
_cell_length_b                   13.2257(4)
_cell_length_c                   15.6462(6)
_cell_measurement_reflns_used    8780
_cell_measurement_temperature    123
_cell_measurement_theta_max      25.3377
_cell_measurement_theta_min      2.7701
_cell_volume                     2267.06(14)
_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
'SHELXL2013 (Sheldrick, 2013), 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 0.978
_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_sigmaI/netI    0.0911
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8439
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         25.70
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    1.022
_exptl_absorpt_correction_T_max  0.745214
_exptl_absorpt_correction_T_min  0.514732
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS, Bruker, 2008b'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.619
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1102
_exptl_crystal_size_max          0.264
_exptl_crystal_size_mid          0.216
_exptl_crystal_size_min          0.134
_platon_squeeze_details
;
The unit cell contains diethyl ether molecules delocalized along tubular 
cavities which have been treated as a diffuse contribution to the overall 
scattering without specific atom positions by SQUEEZE/PLATON.
;
_refine_diff_density_max         0.842
_refine_diff_density_min         -0.822
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     616
_refine_ls_number_reflns         8439
_refine_ls_number_restraints     141
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0933
_refine_ls_R_factor_gt           0.0533
_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^)+(0.0824P)^2^] WHERE P=(FO^2^+2FC^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1293
_refine_ls_wR_factor_ref         0.1454
_reflns_number_gt                5532
_reflns_number_total             8439
_reflns_threshold_expression     i>2\s(i)
_cod_data_source_file            om5013067_si_002.cif
_cod_data_source_block           Compound4f
_cod_database_code               4085809