Cyclic M2(RL)2 Coordination Complexes of 5-(3-[N-tert-Butyl-N-aminoxyl]phenyl)pyrimidine with Paramagnetic Transition Metal Dications
Martha Baskett; Paul M. Lahti; Armando Paduan-Filho; Nei F. Oliveira; Inorganic Chemistry 44 (2005) 6725–6735; doi:10.1021/ic050435t

data_4309583
_publ_contact_author_address
;
[a]Department of Chemistry, University of Massachusetts,
Amherst, MA  01003 USA
[b]Instituto de Fisica, Universidade de Sao Paulo, S. P., 
Brazil
;
_publ_contact_author_email       'lahti@chem.umass.edu '
_publ_contact_author_fax         '1-413-545-4490 '
_publ_contact_author_name
;
Martha Baskett, Paul M. Lahti,[a] 
Armando Paduan-Filho, Nei F. Oliveira Jr. [b]
;
_publ_contact_author_phone       '1-413-545-4890 '
_publ_section_title
;
Cyclic M2(RL)2 Coordination Complexes of
5-(3-[N-tert-Butyl-N-aminoxyl]phenyl)pyrimidine with Paramagnetic
Transition Metal Dications
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6725
_journal_page_last               6735
_journal_paper_doi               10.1021/ic050435t
_journal_volume                  44
_journal_year                    2005
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C25 H19 Cu1 F12 N2 O5'
_chemical_formula_sum            'C25 H19 Cu F12 N2 O5'
_chemical_formula_weight         718.96
_chemical_melting_point          109.5(5)
_chemical_name_common            MB4147
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2005-05-12T21:41:39-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                91.8560(10)
_cell_angle_beta                 94.6500(10)
_cell_angle_gamma                113.8650(10)
_cell_formula_units_Z            2
_cell_length_a                   10.35900(10)
_cell_length_b                   10.40400(10)
_cell_length_c                   14.8870(2)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    293
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_measurement_wavelength     0.71073
_cell_volume                     1458.69(3)
_computing_cell_refinement       Denzo/HKL
_computing_data_collection       Denzo/HKL
_computing_data_reduction        Denzo/HKL
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.0637107
_diffrn_orient_matrix_UB_12      -0.0760317
_diffrn_orient_matrix_UB_13      0.0353992
_diffrn_orient_matrix_UB_21      0.0085327
_diffrn_orient_matrix_UB_22      0.0721875
_diffrn_orient_matrix_UB_23      0.048789
_diffrn_orient_matrix_UB_31      -0.0844444
_diffrn_orient_matrix_UB_32      0.0105284
_diffrn_orient_matrix_UB_33      -0.030526
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0158
_diffrn_reflns_av_unetI/netI     0.0267
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12802
_diffrn_reflns_theta_full        13.75
_diffrn_reflns_theta_max         27.9
_diffrn_reflns_theta_min         4.1
_exptl_absorpt_coefficient_mu    0.864
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.637
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.29
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     594
_refine_ls_number_reflns         6921
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0326
_refine_ls_shift/su_max          0.514
_refine_ls_shift/su_mean         0.021
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0455P)^2^+0.3855P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0813
_refine_ls_wR_factor_ref         0.0874
_reflns_number_gt                5864
_reflns_number_total             6921
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050435tsi20050701_125844.cif
_cod_data_source_block           '_Baskett_Cu_Model-Complex_293K'
_cod_depositor_comments
;
The following automatic conversions were performed:
_chemical_melting_point value '109-110' changed to '109.5(5)' - took
average value and fixed precision.
Automatic conversion script
Id: cif_fix_values 1391 2010-09-07 12:51:13Z saulius 
;
_cod_original_cell_volume        1458.73(3)
_cod_original_formula_sum        'C25 H19 Cu1 F12 N2 O5'
_cod_database_code               4309583