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_4309580
_publ_contact_author_address
;
[a]Department of Chemistry, University of Massachusetts,
Amherst, MA  01003 USA
[b]Instituto de Fisica, Universidade de S\~ao 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_formula_sum            'C48 H36 Cu2 F24 N6 O10'
_chemical_formula_weight         1439.91
_chemical_melting_point          105.0(10)
_chemical_name_systematic
; 
 ? 
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                76.6264(6)
_cell_angle_beta                 81.6717(6)
_cell_angle_gamma                82.5520(9)
_cell_formula_units_Z            2
_cell_length_a                   9.6557(2)
_cell_length_b                   16.0424(3)
_cell_length_c                   19.6212(4)
_cell_measurement_reflns_used    9877
_cell_measurement_temperature    299(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      4.08
_cell_volume                     2911.11(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      299(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Nonius KappaCCD area detector'
_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  0.0324
_diffrn_reflns_av_sigmaI/netI    0.0576
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            18349
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         4.08
_exptl_absorpt_coefficient_mu    0.867
_exptl_absorpt_correction_T_max  0.9787
_exptl_absorpt_correction_T_min  0.4778
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.643
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          1.00
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.808
_refine_diff_density_min         -0.739
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     799
_refine_ls_number_reflns         10202
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.1111
_refine_ls_R_factor_gt           0.0793
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0876P)^2^+7.8668P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1932
_refine_ls_wR_factor_ref         0.2140
_reflns_number_gt                7210
_reflns_number_total             10202
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050435tsi20050701_125819_1.cif
_cod_data_source_block           Baskett_Cu_Complex_299K
_cod_depositor_comments
;
The following automatic conversions were performed:
_chemical_melting_point value '104-106' changed to '105.0(10)' - took
average value and fixed precision.
Automatic conversion script
Id: cif_fix_values 1391 2010-09-07 12:51:13Z saulius 

The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4309580