Coordination Behavior of Bidentate Bis(carbenes) at Alkali Metal Bis(trimethylsilyl)amides
Westerhausen, Matthias; Koch, Alexander; Görls, Helmar; Krieck, Sven; Dalton Trans.  (2017) –; doi:10.1039/C7DT01538K

data_7043402
_publ_section_title
;
 Coordination Behavior of Bidentate Bis(carbenes) at Alkali Metal
 Bis(trimethylsilyl)amides
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01538K
_journal_year                    2017
_chemical_formula_moiety         'C74 H116 K2 N10 Si4, 2(C7 H8)'
_chemical_formula_sum            'C88 H132 K2 N10 Si4'
_chemical_formula_weight         1520.60
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2017-04-27 deposited with the CCDC.
2017-06-21 downloaded from the CCDC.
;
_cell_angle_alpha                92.514(1)
_cell_angle_beta                 103.129(1)
_cell_angle_gamma                100.373(1)
_cell_formula_units_Z            1
_cell_length_a                   11.8026(2)
_cell_length_b                   12.4884(3)
_cell_length_c                   16.4591(2)
_cell_measurement_reflns_used    17648
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.95
_cell_volume                     2314.86(7)
_computing_cell_refinement       DENZO
_computing_data_collection       COLLECT
_computing_data_reduction        DENZO
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi- + omega-scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0199
_diffrn_reflns_av_sigmaI/netI    0.0295
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17648
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.95
_exptl_absorpt_coefficient_mu    0.200
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6979
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker-AXS, 2002'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.091
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.045
_exptl_crystal_size_mid          0.038
_exptl_crystal_size_min          0.028
_refine_diff_density_max         0.603
_refine_diff_density_min         -0.359
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     570
_refine_ls_number_reflns         10278
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0529
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0264P)^2^+1.9822P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1161
_refine_ls_wR_factor_ref         0.1206
_reflns_number_gt                9200
_reflns_number_total             10278
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7dt01538k2.cif
_cod_data_source_block           FO5751
_cod_database_code               7043402