Synthesis, crystal structures and magnetic properties of six coordination compounds constructed with pyridine iminomethyl‒TEMPO radicals and [M(hfac)2] (M = CuII and MnII)
Gao, Yan-Li; Nishihara, Sadafumi; Inoue, Katsuya; CrystEngComm 20 (2018) 2961–; doi:10.1039/C8CE00061A

data_7230624
_publ_section_title
;
 Synthesis, crystal structures and magnetic properties of six coordination
 compounds constructed with pyridine iminomethyl--TEMPO radicals and
 [M(hfac)2] (M = CuII and MnII)
;
_journal_issue                   21
_journal_name_full               CrystEngComm
_journal_page_first              2961
_journal_paper_doi               10.1039/C8CE00061A
_journal_volume                  20
_journal_year                    2018
_chemical_formula_sum            'C25 H24 F12 Mn N3 O5'
_chemical_formula_weight         729.41
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc1yv4xv
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2018-04-03 deposited with the CCDC.
2018-05-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.481(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.8814(7)
_cell_length_b                   14.4685(11)
_cell_length_c                   23.2516(17)
_cell_measurement_reflns_used    9895
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.15
_cell_measurement_theta_min      2.80
_cell_volume                     3268.8(4)
_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-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.984
_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  0.0317
_diffrn_reflns_av_unetI/netI     0.0206
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            63692
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.328
_diffrn_reflns_theta_min         2.802
_exptl_absorpt_coefficient_mu    0.509
_exptl_absorpt_correction_T_max  0.850
_exptl_absorpt_correction_T_min  0.793
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_description       block
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.160
_refine_diff_density_max         0.986
_refine_diff_density_min         -0.590
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     428
_refine_ls_number_reflns         8029
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0792
_refine_ls_R_factor_gt           0.0618
_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^)+(0.1064P)^2^+2.1484P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1801
_refine_ls_wR_factor_ref         0.1960
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6178
_reflns_number_total             8029
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce00061a1.cif
_cod_data_source_block           8
_cod_depositor_comments
'Adding full bibliography for 7230622--7230627.cif.'
_cod_database_code               7230624
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.905
_shelx_estimated_absorpt_t_max   0.923
_shelx_res_checksum              8862