'Janus-type' organopotassium chemistry observed in deprotonation of mesoionic imidazolium aminides and amino N-heterocyclic carbenes: coordination and organometallic polymers
Andreas A. Danopoulos; Pierre Braunstein; Chem.Commun. 50 (2014) 3055–; doi:10.1039/c3cc49517e

data_7112081
_publ_section_title
;
 'Janus-type' organopotassium chemistry observed in deprotonation of
 mesoionic imidazolium aminides and amino N-heterocyclic carbenes:
 coordination and organometallic polymers
;
_journal_name_full               Chem.Commun.
_journal_page_first              3055
_journal_paper_doi               10.1039/c3cc49517e
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C101 H142 K3 N6 O4'
_chemical_formula_sum            'C101 H142 K3 N6 O4'
_chemical_formula_weight         1621.51
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.187(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.7003(3)
_cell_length_b                   15.9846(5)
_cell_length_c                   32.2059(10)
_cell_measurement_reflns_used    9976
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      66.54
_cell_measurement_theta_min      2.83
_cell_volume                     5340.5(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_sigmaI/netI    0.0298
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            34275
_diffrn_reflns_theta_full        66.63
_diffrn_reflns_theta_max         66.63
_diffrn_reflns_theta_min         3.11
_exptl_absorpt_coefficient_mu    1.484
_exptl_absorpt_correction_T_max  0.7557
_exptl_absorpt_correction_T_min  0.5241
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.008
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1758
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_platon_squeeze_details
;
 The residual electron density was assigned to a molecule of the
 pentane solvent [108/4 = 27 e per asymmetric unit; one molecule of
 C5H12 would give 42e].
;
_refine_diff_density_max         0.683
_refine_diff_density_min         -0.652
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         9316
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0904
_refine_ls_R_factor_gt           0.0806
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0924P)^2^+6.7237P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2093
_refine_ls_wR_factor_ref         0.2156
_reflns_number_gt                7800
_reflns_number_total             9316
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c3cc49517e2.cif
_cod_data_source_block           complex14
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7112081