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_7716629
_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            'C23.5 H23 Cl1.5 Cu F12 N4 O6'
_chemical_formula_weight         802.17
_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   mixed
_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                   22.8425(9)
_cell_length_b                   45.5319(16)
_cell_length_c                   12.9843(5)
_cell_measurement_reflns_used    6389
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      19.91
_cell_measurement_theta_min      2.25
_cell_volume                     13504.5(9)
_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      250(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0600
_diffrn_reflns_av_unetI/netI     0.0973
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       61
_diffrn_reflns_limit_k_min       -54
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            34363
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.709
_diffrn_reflns_theta_min         1.789
_exptl_absorpt_coefficient_mu    0.874
_exptl_absorpt_correction_T_max  0.2761
_exptl_absorpt_correction_T_min  0.2286
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_description       block
_exptl_crystal_F_000             6440
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.283
_refine_diff_density_min         -0.220
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details
; 
 Flack x determined using 1331 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.007(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.777
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         8342
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.777
_refine_ls_R_factor_all          0.1127
_refine_ls_R_factor_gt           0.0419
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0476P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0833
_refine_ls_wR_factor_ref         0.0989
_reflns_Friedel_coverage         0.833
_reflns_Friedel_fraction_full    0.947
_reflns_Friedel_fraction_max     0.906
_reflns_number_gt                3791
_reflns_number_total             8342
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01861c2.cif
_cod_data_source_block           z512as
_cod_depositor_comments
'Adding full bibliography for 7716620--7716632.cif.'
_cod_original_formula_sum        'C23.50 H23 Cl1.50 Cu F12 N4 O6'
_cod_database_code               7716629
_shelx_shelxl_version_number     2019/3
_shelx_res_checksum              5236
_shelx_hkl_checksum              26305