The <i>cis</i>/<i>trans</i> conformation approach for tuning the magnetic coupling in a diradical: isolation of pure pyridine-based diradical dianions.
Sun, Qiang; Liu, Min; Ruan, Huapeng; Chen, Chao; Zhao, Yue; Tan, Gengwen; Wang, Xinping; Chemical communications (Cambridge, England) 58 (2022) 1708–1711; doi:10.1039/d1cc05661a

data_7129482
_publ_section_title
;
 The <i>cis</i>/<i>trans</i> conformation approach for tuning the magnetic
 coupling in a diradical: isolation of pure pyridine-based diradical
 dianions.
;
_journal_issue                   11
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1708
_journal_page_last               1711
_journal_paper_doi               10.1039/d1cc05661a
_journal_volume                  58
_journal_year                    2022
_chemical_formula_moiety         'C37 H44 K N O2'
_chemical_formula_sum            'C37 H44 K N O2'
_chemical_formula_weight         573.83
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-03-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-03-20 deposited with the CCDC.	2021-12-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.153(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5553(9)
_cell_length_b                   17.2021(14)
_cell_length_c                   17.3420(13)
_cell_measurement_reflns_used    5645
_cell_measurement_temperature    193
_cell_measurement_theta_max      53.236
_cell_measurement_theta_min      3.221
_cell_volume                     3293.8(5)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193.02
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0890
_diffrn_reflns_av_unetI/netI     0.0923
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22732
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         53.961
_diffrn_reflns_theta_min         3.222
_exptl_absorpt_coefficient_mu    1.077
_exptl_absorpt_correction_T_max  0.7506
_exptl_absorpt_correction_T_min  0.4652
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1611 before and 0.0869 after correction.
The Ratio of minimum to maximum transmission is 0.6198.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear dark blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.157
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.380
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         6005
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.1284
_refine_ls_R_factor_gt           0.0679
_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^)+(0.1033P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1802
_refine_ls_wR_factor_ref         0.2134
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3408
_reflns_number_total             6005
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc05661a2.cif
_cod_data_source_block           trans
_cod_depositor_comments
'Adding full bibliography for 7129481--7129483.cif.'
_cod_database_code               7129482
_shelx_shelxl_version_number     2018/1
_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. Uiso/Uaniso restraints and constraints
C35 \\sim C35A: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
3. Rigid body (RIGU) restrains
 C30, C31, C32, C33, O2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C34, C36, C37, O1, C35
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C34, C36, C37, O1, C35A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Sof(H34C)=Sof(H34D)=Sof(H36C)=Sof(H36D)=Sof(C35A)=Sof(H35C)=Sof(H35D)=1-FVAR(1)
 Sof(H34A)=Sof(H34B)=Sof(H36A)=Sof(H36B)=Sof(C35)=Sof(H35A)=Sof(H35B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,
 H34B), C34(H34C,H34D), C36(H36A,H36B), C36(H36C,H36D), C37(H37A,H37B),
 C35(H35A,H35B), C35A(H35C,H35D)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C6(H6), C8(H8), C10(H10), C14(H14), C16(H16),
 C23(H23), C25(H25)
5.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C27(H27A,H27B,
 H27C), C28(H28A,H28B,H28C), C29(H29C,H29A,H29B)
;
_shelx_res_checksum              5556
_shelx_hkl_checksum              13749
_olex2_submission_special_instructions 'No special instructions were received'