A Copper-Nitroxide Adduct Exhibiting Separate Single Crystal-to-Single Crystal Polymerization-Depolymerization and Spin Crossover Transitions.
Ovcharenko, Victor; Fokin, Sergey; Chubakova, Elvina; Romanenko, Galina; Bogomyakov, Artem; Dobrokhotova, Zhanna; Lukzen, Nikita; Morozov, Vitaly; Petrova, Marina; Petrova, Maria; Zueva, Ekaterina; Rozentsveig, Igor; Rudyakova, Elena; Levkovskaya, Galina; Sagdeev, Renad; Inorganic chemistry 55 (2016) 5853–5861; doi:10.1021/acs.inorgchem.6b00140

data_4347422
_publ_section_title
;
 A Copper-Nitroxide Adduct Exhibiting Separate Single Crystal-to-Single
 Crystal Polymerization-Depolymerization and Spin Crossover Transitions.
;
_journal_issue                   12
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5853
_journal_page_last               5861
_journal_paper_doi               10.1021/acs.inorgchem.6b00140
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C28.5 H29.5 Cu1.25 F15 N4 O7'
_chemical_formula_weight         904.48
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                108.5610(10)
_cell_angle_beta                 91.7480(10)
_cell_angle_gamma                101.5470(10)
_cell_formula_units_Z            4
_cell_length_a                   13.6618(3)
_cell_length_b                   16.5333(3)
_cell_length_c                   17.3793(3)
_cell_measurement_reflns_used    9997
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      27.14
_cell_measurement_theta_min      2.24
_cell_volume                     3627.23(12)
_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-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      140(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.990
_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  0.0597
_diffrn_reflns_av_unetI/netI     0.0676
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            60956
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.096
_diffrn_reflns_theta_min         1.332
_exptl_absorpt_coefficient_mu    0.871
_exptl_absorpt_correction_T_max  0.5193
_exptl_absorpt_correction_T_min  0.4475
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            dark
_exptl_crystal_density_diffrn    1.656
_exptl_crystal_description       bulk
_exptl_crystal_F_000             1823
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.004
_refine_diff_density_min         -0.702
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.945
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1105
_refine_ls_number_reflns         17484
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.945
_refine_ls_R_factor_all          0.0751
_refine_ls_R_factor_gt           0.0464
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0653P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1097
_refine_ls_wR_factor_ref         0.1232
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11456
_reflns_number_total             17484
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00140_si_001.cif
_cod_data_source_block           111s
_cod_original_formula_sum        'C28.50 H29.50 Cu1.25 F15 N4 O7'
_cod_database_code               4347422
_shelx_estimated_absorpt_t_min   sadabs
_shelxl_version_number           2014/6
_shelx_res_checksum              15316