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_4123510
_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_sum            'C54 H55 Cl2 F N3 Sb'
_chemical_formula_weight         957.66
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                91.395(3)
_cell_angle_beta                 106.593(3)
_cell_angle_gamma                108.180(3)
_cell_formula_units_Z            2
_cell_length_a                   11.5206(6)
_cell_length_b                   11.5256(6)
_cell_length_c                   19.7753(10)
_cell_measurement_reflns_used    9894
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.12
_cell_measurement_theta_min      2.28
_cell_volume                     2372.2(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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0436
_diffrn_reflns_av_unetI/netI     0.0459
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            80746
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.998
_diffrn_reflns_theta_min         1.874
_exptl_absorpt_coefficient_mu    0.737
_exptl_absorpt_correction_T_max  0.7466
_exptl_absorpt_correction_T_min  0.6816
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_description       block
_exptl_crystal_F_000             988
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.639
_refine_diff_density_min         -0.738
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     581
_refine_ls_number_reflns         16433
_refine_ls_number_restraints     91
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0389
_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^)+(0.0419P)^2^+0.9048P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0856
_refine_ls_wR_factor_ref         0.0951
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12674
_reflns_number_total             16433
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b00959_si_002.cif
_cod_data_source_block           ah087c
_cod_database_code               4123510
_shelx_estimated_absorpt_t_min   0.815
_shelx_estimated_absorpt_t_max   0.917
_shelxl_version_number           2013-4
_shelx_res_checksum              98506
_shelx_hkl_checksum              73734