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_7230626
_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            'C20 H23 Cu0.5 F6 N3 O3'
_chemical_formula_weight         499.18
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/ccdc.csd.cc1yxpl4
_audit_creation_method           SHELXL-97
_audit_update_record
;
2018-04-03 deposited with the CCDC.
2018-05-11 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.3979(7)
_cell_length_b                   25.7808(11)
_cell_length_c                   10.7851(4)
_cell_measurement_reflns_used    6520
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.38
_cell_measurement_theta_min      2.30
_cell_volume                     4559.4(3)
_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-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0478
_diffrn_reflns_av_sigmaI/netI    0.0206
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            50672
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.76
_exptl_absorpt_coefficient_mu    0.579
_exptl_absorpt_correction_T_max  0.9182
_exptl_absorpt_correction_T_min  0.8930
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2052
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.490
_refine_diff_density_min         -1.431
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         4103
_refine_ls_number_restraints     70
_refine_ls_restrained_S_all      1.139
_refine_ls_R_factor_all          0.1091
_refine_ls_R_factor_gt           0.0965
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1683P)^2^+23.2197P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2659
_refine_ls_wR_factor_ref         0.2823
_reflns_number_gt                3468
_reflns_number_total             4103
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8ce00061a1.cif
_cod_data_source_block           5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7230622--7230627.cif.
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_cod_original_sg_symbol_H-M      Pnma
_cod_original_formula_sum        'C20 H23 Cu0.50 F6 N3 O3'
_cod_database_code               7230626