Stabilization of a Nitroxide with a β-Hydrogen by Metals: Structure and Magnetic Properties of Adducts of N-Oxy-N-tert-butyl-(2-pyridyl)phenylmethanamine with Mn(II), Ni(II), and Co(II) Hexafluoroacetylacetonates
Frederick A. Villamena; Michael H. Dickman; DeLanson R. Crist; Inorganic Chemistry 37 (1998) 1454–1457; doi:10.1021/ic971215l

data_4322728
_publ_section_title
;
 Stabilization of a Nitroxide with a \b-Hydrogen by Metals: Structure and
 Magnetic Properties of Adducts of
 N-Oxy-N-tert-butyl-(2-pyridyl)phenylmethanamine with Mn(II), Ni(II), and
 Co(II) Hexafluoroacetylacetonates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1454
_journal_page_last               1457
_journal_paper_doi               10.1021/ic971215l
_journal_volume                  37
_journal_year                    1998
_chemical_compound_source        synthesized
_chemical_formula_sum            'C26 H21 F12 Mn N2 O5'
_chemical_formula_weight         724.39
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                91.2870(10)
_cell_angle_beta                 100.4090(10)
_cell_angle_gamma                101.1960(10)
_cell_formula_units_Z            2
_cell_length_a                   7.9958(2)
_cell_length_b                   11.6007(2)
_cell_length_c                   17.1049(4)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      30.55
_cell_measurement_theta_min      1.79
_cell_volume                     1528.06(6)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      170(2)
_diffrn_measurement_device       'Siemens SMART CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_sigmaI/netI    0.0339
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            14996
_diffrn_reflns_theta_max         30.55
_diffrn_reflns_theta_min         1.79
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    0.543
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.574
_exptl_crystal_density_meas      ?
_exptl_crystal_description       Irregular
_exptl_crystal_F_000             728
_exptl_crystal_size_max          .34
_exptl_crystal_size_mid          .30
_exptl_crystal_size_min          .18
_refine_diff_density_max         0.575
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.086
_refine_ls_goodness_of_fit_obs   1.104
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     508
_refine_ls_number_reflns         8266
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_restrained_S_obs      1.104
_refine_ls_R_factor_all          0.0699
_refine_ls_R_factor_obs          0.0571
_refine_ls_shift/esd_max         0.009
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0365P)^2^+1.7600P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1320
_refine_ls_wR_factor_obs         0.1229
_reflns_number_observed          6992
_reflns_number_total             8266
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic971215l_2.cif
_cod_data_source_block           mnrm
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0365P)^2^+1.7600P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0365P)^2^+1.7600P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4322728