Solvent-controlled solid-state phase transitions of a heterospin Cu(II) complex with imidazolyl-substituted nitronyl nitroxide.
Smirnova, Kristina A.; Golomolzina, Irina V.; Romanenko, Galina V.; Fokin, Sergey V.; Tolstikov, Svyatoslav E.; Letyagin, Gleb A.; Chernavin, Platon A.; Bogomyakov, Artem S.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 13119–13128; doi:10.1039/d4dt01861c

data_7716620
_publ_section_title
;
 Solvent-controlled solid-state phase transitions of a heterospin Cu(II)
 complex with imidazolyl-substituted nitronyl nitroxide.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13119
_journal_page_last               13128
_journal_paper_doi               10.1039/d4dt01861c
_journal_volume                  53
_journal_year                    2024
_chemical_formula_sum            'C25 H27 Cu F12 N4 O6.5'
_chemical_formula_weight         779.04
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2024-04-23 deposited with the CCDC.	2024-07-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   22.8465(15)
_cell_length_b                   45.601(3)
_cell_length_c                   12.9362(8)
_cell_measurement_reflns_used    5667
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      61.53
_cell_measurement_theta_min      3.88
_cell_volume                     13477.2(15)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.988
_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  0.1014
_diffrn_reflns_av_unetI/netI     0.0743
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -54
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15750
_diffrn_reflns_point_group_measured_fraction_full 0.876
_diffrn_reflns_point_group_measured_fraction_max 0.873
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.854
_diffrn_reflns_theta_min         4.045
_exptl_absorpt_coefficient_mu    1.945
_exptl_absorpt_correction_T_max  0.3447
_exptl_absorpt_correction_T_min  0.1842
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            dark_green
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_description       plate
_exptl_crystal_F_000             6304
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.654
_refine_diff_density_min         -0.420
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details
; 
 Flack x determined using 1280 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.00(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         5350
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0901
_refine_ls_R_factor_gt           0.0743
_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^)+(0.1403P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1958
_refine_ls_wR_factor_ref         0.2100
_reflns_Friedel_coverage         0.688
_reflns_Friedel_fraction_full    0.750
_reflns_Friedel_fraction_max     0.748
_reflns_number_gt                3989
_reflns_number_total             5350
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01861c2.cif
_cod_data_source_block           512bs
_cod_depositor_comments
'Adding full bibliography for 7716620--7716632.cif.'
_cod_original_cell_volume        13477.3(15)
_cod_original_formula_sum        'C25 H27 Cu F12 N4 O6.50'
_cod_database_code               7716620
_shelx_shelxl_version_number     2019/3
_shelx_res_checksum              58922
_shelx_hkl_checksum              29277