Synthesis, structural characterization and electrochemical and magnetic studies of M(hfac)<sub>2</sub> (M = Cu<sup>II</sup>, Co<sup>II</sup>) and Nd(hfac)<sub>3</sub> complexes of 4-amino-TEMPO.
Navarro, Yolanda; Guedes, Guilherme P.; Cano, Joan; Ocón, Pilar; Iglesias, María José; Lloret, Francisco; López-Ortiz, Fernando; Dalton transactions (Cambridge, England : 2003) 49 (2020) 6280–6294; doi:10.1039/d0dt00541j

data_7704121
_publ_section_title
;
 Synthesis, structural characterization and electrochemical and magnetic
 studies of M(hfac)<sub>2</sub> (M = Cu<sup>II</sup>, Co<sup>II</sup>) and
 Nd(hfac)<sub>3</sub> complexes of 4-amino-TEMPO.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6280
_journal_page_last               6294
_journal_paper_doi               10.1039/d0dt00541j
_journal_volume                  49
_journal_year                    2020
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C28 H40 Cu F12 N4 O6'
_chemical_formula_sum            'C28 H40 Cu F12 N4 O6'
_chemical_formula_weight         820.19
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2020-01-16 deposited with the CCDC.	2020-04-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.7940(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.0543(3)
_cell_length_b                   11.8676(3)
_cell_length_c                   12.4149(3)
_cell_measurement_reflns_used    9216
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.37
_cell_measurement_theta_min      3.60
_cell_volume                     1755.14(8)
_computing_cell_refinement       'Bruker Smart (Bruker AXS, 2007)'
_computing_data_collection       'Bruker Smart (Bruker AXS, 2007)'
_computing_data_reduction        'Bruker Saint (Bruker AXS, 2007)'
_computing_molecular_graphics    'Mercury (Bruno, 2002)'
_computing_publication_material
'WinGX publication routines (Farrugia, 1999) and publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Apex II CCD'
_diffrn_measurement_method       '\f-\w scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            26297
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.398
_diffrn_reflns_theta_min         3.602
_exptl_absorpt_coefficient_mu    1.881
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.6723
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS, Bruker Analytical X-ray Systems,Inc., Madison WI, 1997.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_description       block
_exptl_crystal_F_000             842
_exptl_crystal_size_max          0.175
_exptl_crystal_size_mid          0.102
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.391
_refine_diff_density_min         -0.276
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details
;
 Flack x determined using 2838 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.003(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         6828
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0275
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0338P)^2^+0.4471P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0639
_refine_ls_wR_factor_ref         0.0656
_reflns_Friedel_coverage         0.876
_reflns_Friedel_fraction_full    0.976
_reflns_Friedel_fraction_max     0.966
_reflns_number_gt                6435
_reflns_number_total             6949
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00541j2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7704121--7704125.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7704121
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.734
_shelx_estimated_absorpt_t_max   0.864
_shelx_res_checksum              16319