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_4133866
_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         '2(Cl6 Sb), C64 H84 N2, 2(C H2 Cl2)'
_chemical_formula_sum            'C66 H88 Cl16 N2 Sb2'
_chemical_formula_weight         1720.08
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-10-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                84.5548(12)
_cell_angle_beta                 89.4723(12)
_cell_angle_gamma                67.0952(12)
_cell_formula_units_Z            1
_cell_length_a                   8.8952(3)
_cell_length_b                   11.4019(4)
_cell_length_c                   20.5690(7)
_cell_measurement_reflns_used    9498
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      70.082
_cell_measurement_theta_min      4.230
_cell_volume                     1912.12(11)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_av_unetI/netI     0.0240
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            45841
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.206
_diffrn_reflns_theta_min         2.159
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    11.044
_exptl_absorpt_correction_T_max  0.3841
_exptl_absorpt_correction_T_min  0.1847
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1132 before and 0.0637 after correction. The Ratio of minimum to maximum transmission is 0.4809. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_description       needle
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.499
_exptl_crystal_size_mid          0.128
_exptl_crystal_size_min          0.058
_refine_diff_density_max         1.336
_refine_diff_density_min         -1.290
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     456
_refine_ls_number_reflns         7214
_refine_ls_number_restraints     139
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0348P)^2^+5.0908P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0960
_refine_ls_wR_factor_ref         0.0987
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6691
_reflns_number_total             7214
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b12626_si_002.cif
_cod_data_source_block           memeq
_cod_database_code               4133866
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.567
_shelx_estimated_absorpt_t_min   0.073
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C32-C31 = C32A-C31A
 1.54 with sigma of 0.005
 C28A-C27 \\sim C28-C27
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C28A \\sim C29A \\sim C30A
\\sim C31A \\sim C32A: within 2A with sigma of 0.005 and sigma for terminal
atoms of 0.01
Uanis(C32A) = Uanis(C31A)
Uanis(C33A) = Uanis(Cl8A)
4. Rigid body (RIGU) restrains
 C28, C29, C30, C31, C32, C28A, C29A, C30A, C31A, C32A
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
5. Same fragment restrains
{C28, C29, C30, C31, C32} sigma for 1-2: 0.005, 1-3: 0.04
as
{C28A, C29A, C30A, C31A, C32A}
{Cl7, Cl8, C33} sigma for 1-2: 0.005, 1-3: 0.04
as
{Cl7A, Cl8A, C33A}
6. Others
 Sof(C29A)=Sof(H29C)=Sof(H29D)=Sof(C30A)=Sof(H30C)=Sof(H30D)=Sof(C31A)=
 Sof(H31C)=Sof(H31D)=Sof(C32A)=Sof(H32D)=Sof(H32E)=Sof(H32F)=Sof(Cl7A)=
 Sof(Cl8A)=Sof(C33A)=Sof(H33C)=Sof(H33D)=1-FVAR(1)
 Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(C31)=Sof(H31A)=
 Sof(H31B)=Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=Sof(Cl7)=Sof(Cl8)=Sof(C33)=
 Sof(H33A)=Sof(H33B)=FVAR(1)
 Sof(H27C)=Sof(H27D)=Sof(C28A)=Sof(H28C)=Sof(H28D)=1-FVAR(2)
 Sof(H27A)=Sof(H27B)=Sof(C28)=Sof(H28A)=Sof(H28B)=FVAR(2)
7.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,
 H25B), C27(H27A,H27B), C27(H27C,H27D), C28(H28A,H28B), C29(H29A,H29B),
 C30(H30A,H30B), C31(H31A,H31B), C28A(H28C,H28D), C29A(H29C,H29D), C30A(H30C,
 H30D), C31A(H31C,H31D), C33(H33A,H33B), C33A(H33C,H33D)
7.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C10(H10), C13(H13), C16(H16)
7.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C26(H26A,H26B,
 H26C), C32(H32A,H32B,H32C), C32A(H32D,H32E,H32F)
;
_shelx_res_checksum              36942
_shelx_hkl_checksum              29744
_olex2_submission_special_instructions 'No special instructions were received'