Preparation and Magnetic Properties of Metal-Complexes from N-t-Butyl-N-oxidanyl-2-amino-(nitronyl nitroxide).
Furui, Takanori; Suzuki, Shuichi; Kozaki, Masatoshi; Shiomi, Daisuke; Sato, Kazunobu; Takui, Takeji; Okada, Keiji; Tretyakov, Evgeny V.; Tolstikov, Svyatoslav E.; Romanenko, Galina V.; Ovcharenko, Victor I.; Inorganic chemistry 53 (2014) 802–809; doi:10.1021/ic4020898

data_4337085
_publ_section_title
;
 Preparation and Magnetic Properties of Metal-Complexes from
 N-t-Butyl-N-oxidanyl-2-amino-(nitronyl nitroxide).
;
_journal_issue                   2
_journal_name_full               'Inorganic chemistry'
_journal_page_first              802
_journal_page_last               809
_journal_paper_doi               10.1021/ic4020898
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C21 H23 F12 Mn N3 O7'
_chemical_formula_sum            'C21 H23 F12 Mn N3 O7'
_chemical_formula_weight         712.36
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_audit_creation_date             2009-09-28
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.202(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   25.1960(13)
_cell_length_b                   8.5524(4)
_cell_length_c                   27.5246(16)
_cell_measurement_reflns_used    6797
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      4.0350
_cell_volume                     5931.1(5)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku, 2001)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>,  1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 7.32
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_details
;

scan:

    Number of images: 900

               Slice: -80.0000 - 100.0000

         Image width: 0.2000

            Exp time: 3.0000

       Rotation axis: Phi

               Omega: 0.0000

                 Chi: 0.0000

                 Phi: 0.0000

                 XTD: 55.2872

              2theta: 24.7479

scan:

    Number of images: 300

               Slice: -15.0000 - 45.0000

         Image width: 0.2000

            Exp time: 3.0000

       Rotation axis: Omega

               Omega: 0.0000

                 Chi: 90.0000

                 Phi: 0.0000

                 XTD: 55.2872

              2theta: 24.7479

scan:

    Number of images: 300

               Slice: -15.0000 - 45.0000

         Image width: 0.2000

            Exp time: 3.0000

       Rotation axis: Omega

               Omega: 0.0000

                 Chi: 90.0000

                 Phi: 90.0000

                 XTD: 55.2872

              2theta: 24.7479

scan:

    Number of images: 300

               Slice: -15.0000 - 45.0000

         Image width: 0.2000

            Exp time: 3.0000

       Rotation axis: Omega

               Omega: 0.0000

                 Chi: 90.0000

                 Phi: 180.0000

                 XTD: 55.2872

              2theta: 24.7479

scan:

    Number of images: 300

               Slice: -15.0000 - 45.0000

         Image width: 0.2000

            Exp time: 3.0000

       Rotation axis: Omega

               Omega: 0.0000

                 Chi: 90.0000

                 Phi: 270.0000

                 XTD: 55.2872

              2theta: 24.7479

;
_diffrn_measurement_device       'Mercury CCD (2x2 bin mode)'
_diffrn_measurement_device_details 'AFC7: Eulerian 3-circle'
_diffrn_measurement_device_type  'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method       '\w or \f'
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_av_sigmaI/netI    0.0279
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            21901
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         4.07
_diffrn_source_current           100.0000
_diffrn_source_power             5.0000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.564
_exptl_absorpt_correction_T_max  0.8402
_exptl_absorpt_correction_T_min  0.8143
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Jacobson, 1998)'
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.596
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2872
_exptl_crystal_preparation
'mounted on a glass fiber with epoxy resin and placed in N2 stream at 150(2) K'
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.32
_refine_diff_density_max         1.042
_refine_diff_density_min         -0.750
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         6588
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0755
_refine_ls_R_factor_gt           0.0648
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0594P)^2^+25.1447P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1486
_refine_ls_wR_factor_ref         0.1546
_reflns_number_gt                5797
_reflns_number_total             6588
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4020898_si_002.cif
_cod_data_source_block           Mn-NNtBuNO
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/automatic-downloads/current/ACS/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 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4337085