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_7715914
_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 Co0.11 N3 Ni0.89 O5'
_chemical_formula_weight         759.69
_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                 100.755(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7610(5)
_cell_length_b                   15.6753(6)
_cell_length_c                   27.0721(11)
_cell_measurement_reflns_used    10940
_cell_measurement_temperature    240(2)
_cell_measurement_theta_max      26.8360
_cell_measurement_theta_min      3.3240
_cell_volume                     4486.4(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.999
_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  0.0835
_diffrn_reflns_av_unetI/netI     0.0676
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            89592
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.000
_diffrn_reflns_theta_min         3.005
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.469
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74054
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.125
_exptl_crystal_description       prism
_exptl_crystal_F_000             1636
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.230
_refine_diff_density_min         -0.239
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     494
_refine_ls_number_reflns         13064
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.1117
_refine_ls_R_factor_gt           0.0526
_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^)+(0.0374P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0905
_refine_ls_wR_factor_ref         0.1036
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7633
_reflns_number_total             13064
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00453a2.cif
_cod_data_source_block           nicosqnntempo_240
_cod_depositor_comments
'Adding full bibliography for 7715910--7715918.cif.'
_cod_original_cell_volume        4486.3(3)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7715914
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.835
_shelx_estimated_absorpt_t_max   0.912
_oxdiff_exptl_absorpt_empirical_full_min 0.851
_oxdiff_exptl_absorpt_empirical_full_max 1.382
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              80982