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_7129483
_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         'C41 H52 K N O6'
_chemical_formula_sum            'C41 H52 K N O6'
_chemical_formula_weight         693.93
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_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                 98.184(6)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.7899(16)
_cell_length_b                   20.4638(19)
_cell_length_c                   22.710(2)
_cell_measurement_reflns_used    1082
_cell_measurement_temperature    192.98
_cell_measurement_theta_max      39.083
_cell_measurement_theta_min      2.716
_cell_volume                     9103.4(14)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_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      192.98
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.1608
_diffrn_reflns_av_unetI/netI     0.1407
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            25582
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         53.907
_diffrn_reflns_theta_min         2.717
_exptl_absorpt_coefficient_mu    0.868
_exptl_absorpt_correction_T_max  0.7519
_exptl_absorpt_correction_T_min  0.4412
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1403 before and 0.0687 after correction.
The Ratio of minimum to maximum transmission is 0.5868.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.013
_exptl_crystal_description       block
_exptl_crystal_F_000             2976
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.357
_refine_diff_density_min         -0.566
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.261
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     456
_refine_ls_number_reflns         8269
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.261
_refine_ls_R_factor_all          0.2045
_refine_ls_R_factor_gt           0.1166
_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^)+(0.1300P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2828
_refine_ls_wR_factor_ref         0.3363
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3822
_reflns_number_total             8269
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc05661a2.cif
_cod_data_source_block           cis
_cod_depositor_comments
'Adding full bibliography for 7129481--7129483.cif.'
_cod_original_cell_volume        9103.3(14)
_cod_database_code               7129483
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.881
_shelx_estimated_absorpt_t_min   0.846
_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:
 C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,
 H34B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B),
 C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C8(H8), C10(H10), C14(H14), C16(H16), C23(H23), C25(H25)
2.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(H29A,H29B,H29C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              14547
_shelx_hkl_checksum              77144
_shelx_fab_checksum              37234
_olex2_submission_special_instructions 'No special instructions were received'