Cyclo-Pnicta-triazanes: Biradicaloids - or Zwitterions?
Hinz, Alexander; Schulz, Axel; Villinger, Alexander; Wolter, Jan-Martin; Journal of the American Chemical Society  (2015) 150316134803000–; doi:10.1021/jacs.5b00959

data_4123518
_publ_section_title
;
 Cyclo-Pnicta-triazanes: Biradicaloids - or Zwitterions?
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              150316134803000
_journal_paper_doi               10.1021/jacs.5b00959
_journal_year                    2015
_chemical_formula_moiety         'C52 H58 Li N3 O, C6 H6'
_chemical_formula_sum            'C58 H64 Li N3 O'
_chemical_formula_weight         826.06
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 93.347(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.4666(3)
_cell_length_b                   14.2657(4)
_cell_length_c                   29.3989(8)
_cell_measurement_reflns_used    9949
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      31.21
_cell_measurement_theta_min      2.28
_cell_volume                     4800.8(2)
_computing_cell_refinement       'Bruker Apex V7.51A'
_computing_data_collection       'Bruker Apex V7.51A'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material  SHELXL-2013
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Apex Kappa II-CCD-diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0566
_diffrn_reflns_av_unetI/netI     0.0475
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            71644
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.998
_diffrn_reflns_theta_min         1.587
_exptl_absorpt_coefficient_mu    0.067
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.6835
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.143
_exptl_crystal_description       block
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.490
_exptl_crystal_size_mid          0.420
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.119
_refine_diff_density_min         -0.184
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     649
_refine_ls_number_reflns         12762
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0904
_refine_ls_R_factor_gt           0.0535
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0570P)^2^+1.7937P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1252
_refine_ls_wR_factor_ref         0.1464
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8456
_reflns_number_total             12762
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b00959_si_002.cif
_cod_data_source_block           ah159b
_cod_database_code               4123518
_shelx_estimated_absorpt_t_min   0.968
_shelx_estimated_absorpt_t_max   0.987
_shelxl_version_number           2013-4
_shelx_res_checksum              66904
_shelx_hkl_checksum              81379