Pauli Paramagnetism of Stable Analogues of Pernigraniline Salt Featuring Ladder-Type Constitution.
Ji, Xiaozhou; Xie, Haomiao; Zhu, Congzhi; Zou, Yang; Mu, Anthony U.; Al-Hashimi, Mohammed; Dunbar, Kim R.; Fang, Lei; Journal of the American Chemical Society  (2019) –; doi:10.1021/jacs.9b12626

data_4133867
_publ_section_title
;
 Pauli Paramagnetism of Stable Analogues of Pernigraniline Salt Featuring
 Ladder-Type Constitution.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b12626
_journal_year                    2019
_chemical_formula_moiety         'C62 H78 N2'
_chemical_formula_sum            'C62 H78 N2'
_chemical_formula_weight         851.26
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2016-12-12
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 98.087(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   20.9363(13)
_cell_length_b                   10.6422(7)
_cell_length_c                   11.1562(7)
_cell_measurement_reflns_used    9815
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      19.155
_cell_measurement_theta_min      2.658
_cell_volume                     2461.0(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0865
_diffrn_reflns_av_unetI/netI     0.0277
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            41972
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        19.192
_diffrn_reflns_theta_max         19.192
_diffrn_reflns_theta_min         2.658
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.065
_exptl_absorpt_correction_T_max  0.7443
_exptl_absorpt_correction_T_min  0.5694
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1564 before and 0.0894 after correction.
The Ratio of minimum to maximum transmission is 0.7650.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.149
_exptl_crystal_description       block
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.681
_exptl_crystal_size_mid          0.204
_exptl_crystal_size_min          0.042
_refine_diff_density_max         0.414
_refine_diff_density_min         -0.247
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         2040
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.0826
_refine_ls_R_factor_gt           0.0691
_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^)+(0.0593P)^2^+6.4410P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1573
_refine_ls_wR_factor_ref         0.1689
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1688
_reflns_number_total             2040
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b12626_si_003.cif
_cod_data_source_block           lfb_xj_2
_cod_database_code               4133867
_shelx_estimated_absorpt_t_max   0.997
_shelx_estimated_absorpt_t_min   0.957
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,
 H24B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B),
 C30(H30A,H30B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C7(H7), C10(H10), C14(H14), C15(H15), C16(H16), C17(H17)
2.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C25(H25A,H25B,H25C), C31(H31A,H31B,
 H31C)
;
_shelx_res_checksum              22024
_shelx_hkl_checksum              69282
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'