Valence tautomeric interconversion of bis-dioxolene cobalt complex with imino-pyridine functionalized by TEMPO moiety in solid solutions with isostructural nickel analogue: phase transitions and monocrystal destruction.
Bubnov, Michael P.; Zolotukhin, Alexey A.; Fukin, Georgy K.; Rumyantcev, Roman V.; Bogomyakov, Artem S.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 9151–9160; doi:10.1039/d4dt00453a

data_7715910
_publ_section_title
;
 Valence tautomeric interconversion of bis-dioxolene cobalt complex with
 imino-pyridine functionalized by TEMPO moiety in solid solutions with
 isostructural nickel analogue: phase transitions and monocrystal
 destruction.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9151
_journal_page_last               9160
_journal_paper_doi               10.1039/d4dt00453a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_sum            'C43 H62 Co0.5 N3 Ni0.5 O5'
_chemical_formula_weight         759.77
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2024-02-14 deposited with the CCDC.	2024-04-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.056(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7499(2)
_cell_length_b                   15.7050(3)
_cell_length_c                   26.8932(6)
_cell_measurement_reflns_used    19046
_cell_measurement_temperature    240(2)
_cell_measurement_theta_max      27.4210
_cell_measurement_theta_min      2.0180
_cell_volume                     4456.04(16)
_computing_cell_refinement       'CrysAlisPro 1.171.43.105a (Rigaku OD, 2024)'
_computing_data_collection       'CrysAlisPro 1.171.43.105a (Rigaku OD, 2024)'
_computing_data_reduction        'CrysAlisPro 1.171.43.105a (Rigaku OD, 2024)'
_computing_structure_refinement  SHELXL-2019/3
_computing_structure_solution    SHELXT-2014/5
_diffrn_ambient_temperature      240(2)
_diffrn_detector_area_resol_mean 16.0704
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_unetI/netI     0.0224
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            60877
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         2.016
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.453
_exptl_absorpt_correction_T_max  0.931
_exptl_absorpt_correction_T_min  0.863
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.105a (Rigaku Oxford Diffraction, 2024)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.133
_exptl_crystal_description       prism
_exptl_crystal_F_000             1634
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.330
_exptl_crystal_size_min          0.190
_refine_diff_density_max         0.302
_refine_diff_density_min         -0.255
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     494
_refine_ls_number_reflns         10211
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0351
_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^)+(0.0423P)^2^+0.9003P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0836
_refine_ls_wR_factor_ref         0.0938
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7824
_reflns_number_total             10211
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00453a2.cif
_cod_data_source_block           conisqnntempo_240_1_1
_cod_depositor_comments
'Adding full bibliography for 7715910--7715918.cif.'
_cod_original_cell_volume        4456.03(16)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C43 H62 Co0.50 N3 Ni0.50 O5'
_cod_database_code               7715910
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.833
_shelx_estimated_absorpt_t_max   0.919
_oxdiff_exptl_absorpt_empirical_full_min 0.948
_oxdiff_exptl_absorpt_empirical_full_max 1.112
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              20702