#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/25/4312540.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4312540
loop_
_publ_author_name
'Lora M. Field'
'Paul M. Lahti'
_publ_contact_author_address
;
Department of Chemistry, University of Massachusetts,
Amherst, MA  01003  USA
;
_publ_contact_author_email       'lahti@chem.umass.edu '
_publ_contact_author_fax         '413-545-4490 '
_publ_contact_author_name        'Paul M. Lahti'
_publ_contact_author_phone       '413-545-4890 '
_publ_section_title
;
 Coordination Complexes of
 1-(4-[N-tert-Butyl-N-aminoxyl]phenyl)-1H-1,2,4-triazole with Paramagnetic
 Transition Metal Dications
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7447
_journal_page_last               7454
_journal_paper_doi               10.1021/ic0349050
_journal_volume                  42
_journal_year                    2003
_chemical_compound_source        'Local laboratory'
_chemical_formula_moiety         'C22 H17 Co F12 N4 O5 '
_chemical_formula_sum            'C22 H17 Co F12 N4 O5'
_chemical_formula_weight         704.310
_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'
_audit_creation_method           maXus
_cell_angle_alpha                93.0482(6)
_cell_angle_beta                 91.6094(6)
_cell_angle_gamma                115.4709(10)
_cell_formula_units_Z            2
_cell_length_a                   9.73670(10)
_cell_length_b                   10.5646(2)
_cell_length_c                   14.8865(3)
_cell_measurement_reflns_used    4703
_cell_measurement_temperature    298
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      4.076
_cell_volume                     1378.29(4)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       KappaCCD
_computing_data_reduction
'Denzo and Scalepak (Otwinowski & Minor, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       KappaCCD
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_UB_11      0.10402
_diffrn_orient_matrix_UB_12      0.04573
_diffrn_orient_matrix_UB_13      0.00852
_diffrn_orient_matrix_UB_21      0.03043
_diffrn_orient_matrix_UB_22      0.05918
_diffrn_orient_matrix_UB_23      -0.08138
_diffrn_orient_matrix_UB_31      -0.02322
_diffrn_orient_matrix_UB_32      0.05733
_diffrn_orient_matrix_UB_33      0.02672
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           ' MoK\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0176
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9015
_diffrn_reflns_theta_full        25.04
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         4.12
_exptl_absorpt_coefficient_mu    0.745
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.697
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             704
_exptl_crystal_size_max          1.100
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.862
_refine_diff_density_min         -0.470
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         4833
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0526
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0806P)²+1.4024P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1414
_refine_ls_wR_factor_ref         0.1484
_reflns_number_gt                4289
_reflns_number_total             4833
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0349050si20030730_014852_4.cif
_cod_data_source_block           global
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C22 H17 Co F12 N4 O5 '
_cod_database_code               4312540
loop_
_symmetry_equiv_pos_as_xyz
+X,+Y,+Z
-X,-Y,-Z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.87177(5) 0.39869(4) 0.27476(3) 0.04408(17) Uani 1 1 d . . .
O2 O 0.8861(3) 0.3162(2) 0.39503(15) 0.0515(5) Uani 1 1 d . . .
O1 O 0.6474(2) 0.2465(2) 0.24869(16) 0.0502(5) Uani 1 1 d . . .
N4 N 0.1905(3) 0.4592(3) 0.65233(19) 0.0468(6) Uani 1 1 d . . .
O4 O 1.1044(3) 0.5336(2) 0.28504(17) 0.0556(6) Uani 1 1 d . . .
O3 O 0.9153(3) 0.2375(2) 0.21371(16) 0.0528(5) Uani 1 1 d . . .
O5 O 0.8622(3) 0.4888(2) 0.15787(15) 0.0536(5) Uani 1 1 d . . .
N1 N 0.5243(3) 0.2621(3) 0.23261(18) 0.0497(6) Uani 1 1 d . . .
C14 C 0.8602(3) 0.1899(3) 0.4027(2) 0.0478(7) Uani 1 1 d . . .
N2 N 0.2692(3) 0.3608(3) 0.54640(18) 0.0454(6) Uani 1 1 d . . .
C11 C 0.2174(4) 0.4559(3) 0.5665(2) 0.0479(7) Uani 1 1 d . . .
C21 C 0.9647(4) 0.5954(3) 0.1291(2) 0.0515(8) Uani 1 1 d . . .
C5 C 0.4501(3) 0.2817(3) 0.3085(2) 0.0468(7) Uani 1 1 d . . .
C12 C 0.2286(4) 0.3590(4) 0.6832(2) 0.0573(8) Uani 1 1 d . . .
C8 C 0.3252(3) 0.3298(3) 0.4645(2) 0.0447(7) Uani 1 1 d . . .
C16 C 0.8808(4) 0.1234(3) 0.2468(2) 0.0503(7) Uani 1 1 d . . .
C9 C 0.4197(4) 0.2625(3) 0.4678(2) 0.0501(7) Uani 1 1 d . . .
N3 N 0.2768(4) 0.2963(3) 0.6224(2) 0.0604(8) Uani 1 1 d . . .
C19 C 1.1709(4) 0.6331(4) 0.2378(2) 0.0544(8) Uani 1 1 d . . .
F2 F 0.6789(3) 0.0742(3) 0.50627(18) 0.0937(8) Uani 1 1 d . . .
C10 C 0.4809(4) 0.2392(3) 0.3902(2) 0.0502(7) Uani 1 1 d . . .
C13 C 0.8262(4) 0.1414(4) 0.4974(3) 0.0596(9) Uani 1 1 d . . .
C17 C 0.8638(5) 0.0006(4) 0.1800(3) 0.0652(10) Uani 1 1 d . . .
F10 F 0.8452(5) 0.5426(4) -0.01626(17) 0.1198(12) Uani 1 1 d . . .
F6 F 0.9169(5) 0.0383(3) 0.10360(19) 0.1141(11) Uani 1 1 d . . .
F1 F 0.8802(4) 0.2439(3) 0.55982(17) 0.1154(12) Uani 1 1 d . . .
F3 F 0.8798(5) 0.0503(4) 0.5182(2) 0.1284(13) Uani 1 1 d . . .
F5 F 0.9473(4) -0.0647(3) 0.2106(2) 0.1116(10) Uani 1 1 d . . .
C15 C 0.8539(4) 0.0912(4) 0.3358(2) 0.0584(8) Uani 1 1 d . . .
C6 C 0.3513(4) 0.3459(4) 0.3061(2) 0.0613(9) Uani 1 1 d . . .
F11 F 0.8149(5) 0.6936(4) 0.0638(2) 0.1153(12) Uani 1 1 d . . .
C20 C 1.1117(4) 0.6729(4) 0.1643(3) 0.0619(9) Uani 1 1 d . . .
C7 C 0.2885(4) 0.3688(4) 0.3840(3) 0.0611(9) Uani 1 1 d . . .
C22 C 0.9153(5) 0.6446(5) 0.0444(3) 0.0725(11) Uani 1 1 d . . .
F9 F 1.3867(4) 0.8510(4) 0.2576(4) 0.176(2) Uani 1 1 d . . .
F12 F 1.0266(5) 0.7428(6) 0.0077(3) 0.197(3) Uani 1 1 d . . .
F4 F 0.7287(4) -0.0967(4) 0.1740(3) 0.1530(19) Uani 1 1 d . . .
C4 C 0.4590(4) 0.2331(4) 0.1358(2) 0.0659(10) Uani 1 1 d . . .
F8 F 1.4204(4) 0.6728(5) 0.2130(4) 0.172(2) Uani 1 1 d . . .
F7 F 1.3788(4) 0.7041(4) 0.3446(3) 0.1374(14) Uani 1 1 d . . .
C2 C 0.4815(6) 0.3736(6) 0.0991(3) 0.0930(15) Uani 1 1 d . . .
C18 C 1.3410(5) 0.7199(5) 0.2622(4) 0.0834(13) Uani 1 1 d . . .
C3 C 0.2916(5) 0.1303(6) 0.1345(4) 0.1074(19) Uani 1 1 d . . .
C1 C 0.5498(6) 0.1724(7) 0.0818(3) 0.0996(17) Uani 1 1 d . . .
H11 H 0.2023 0.5126 0.5254 0.058 Uiso 1 1 calc R . .
H12 H 0.2210 0.3369 0.7431 0.069 Uiso 1 1 calc R . .
H9 H 0.4414 0.2333 0.5221 0.060 Uiso 1 1 calc R . .
H10 H 0.5444 0.1940 0.3925 0.060 Uiso 1 1 calc R . .
H15 H 0.8308 0.0003 0.3509 0.070 Uiso 1 1 calc R . .
H6 H 0.3275 0.3735 0.2518 0.074 Uiso 1 1 calc R . .
H20 H 1.1734 0.7547 0.1379 0.074 Uiso 1 1 calc R . .
H7 H 0.2217 0.4105 0.3819 0.073 Uiso 1 1 calc R . .
H2A H 0.4239 0.4123 0.1325 0.139 Uiso 1 1 calc R . .
H2B H 0.4471 0.3582 0.0366 0.139 Uiso 1 1 calc R . .
H2C H 0.5876 0.4380 0.1051 0.139 Uiso 1 1 calc R . .
H3A H 0.2372 0.1723 0.1682 0.161 Uiso 1 1 calc R . .
H3B H 0.2817 0.0462 0.1612 0.161 Uiso 1 1 calc R . .
H3C H 0.2500 0.1074 0.0734 0.161 Uiso 1 1 calc R . .
H1A H 0.6548 0.2396 0.0841 0.149 Uiso 1 1 calc R . .
H1B H 0.5100 0.1512 0.0204 0.149 Uiso 1 1 calc R . .
H1C H 0.5421 0.0879 0.1070 0.149 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_diffrn_radiation_wavelength_id
all
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O5 Co1 O2 177.64(9) . . ?
O5 Co1 O4 86.73(9) . . ?
O2 Co1 O4 91.75(9) . . ?
O5 Co1 O1 90.77(9) . . ?
O2 Co1 O1 91.00(9) . . ?
O4 Co1 O1 171.16(9) . . ?
O5 Co1 O3 95.54(9) . . ?
O2 Co1 O3 86.28(9) . . ?
O4 Co1 O3 90.90(9) . . ?
O1 Co1 O3 80.89(9) . . ?
O5 Co1 N4 90.49(10) . 2_666 ?
O2 Co1 N4 87.82(10) . 2_666 ?
O4 Co1 N4 94.14(10) . 2_666 ?
O1 Co1 N4 94.36(9) . 2_666 ?
O3 Co1 N4 172.35(9) . 2_666 ?
C14 O2 Co1 124.3(2) . . ?
N1 O1 Co1 129.64(18) . . ?
C11 N4 C12 102.6(3) . . ?
C11 N4 Co1 127.9(2) . 2_666 ?
C12 N4 Co1 129.1(2) . 2_666 ?
C19 O4 Co1 126.0(2) . . ?
C16 O3 Co1 122.9(2) . . ?
C21 O5 Co1 126.9(2) . . ?
O1 N1 C5 116.4(3) . . ?
O1 N1 C4 117.2(3) . . ?
C5 N1 C4 125.5(3) . . ?
O2 C14 C15 128.0(3) . . ?
O2 C14 C13 114.6(3) . . ?
C15 C14 C13 117.4(3) . . ?
C11 N2 N3 109.2(3) . . ?
C11 N2 C8 130.3(3) . . ?
N3 N2 C8 120.2(2) . . ?
N4 C11 N2 110.9(3) . . ?
O5 C21 C20 128.7(3) . . ?
O5 C21 C22 113.8(3) . . ?
C20 C21 C22 117.5(3) . . ?
C10 C5 C6 118.4(3) . . ?
C10 C5 N1 118.3(3) . . ?
C6 C5 N1 123.3(3) . . ?
N3 C12 N4 114.8(3) . . ?
C7 C8 C9 120.6(3) . . ?
C7 C8 N2 120.5(3) . . ?
C9 C8 N2 119.0(3) . . ?
O3 C16 C15 128.6(3) . . ?
O3 C16 C17 115.5(3) . . ?
C15 C16 C17 115.9(3) . . ?
C10 C9 C8 119.4(3) . . ?
C12 N3 N2 102.5(3) . . ?
O4 C19 C20 128.3(3) . . ?
O4 C19 C18 115.5(3) . . ?
C20 C19 C18 116.2(4) . . ?
C9 C10 C5 121.3(3) . . ?
F1 C13 F2 107.3(4) . . ?
F1 C13 F3 106.7(4) . . ?
F2 C13 F3 104.3(3) . . ?
F1 C13 C14 113.3(3) . . ?
F2 C13 C14 111.2(3) . . ?
F3 C13 C14 113.4(3) . . ?
F4 C17 F6 113.1(4) . . ?
F4 C17 F5 103.1(4) . . ?
F6 C17 F5 103.1(3) . . ?
F4 C17 C16 112.1(3) . . ?
F6 C17 C16 114.0(3) . . ?
F5 C17 C16 110.5(4) . . ?
C14 C15 C16 122.3(3) . . ?
C7 C6 C5 120.4(3) . . ?
C21 C20 C19 122.3(3) . . ?
C8 C7 C6 119.8(3) . . ?
F10 C22 F12 108.1(4) . . ?
F10 C22 F11 104.6(4) . . ?
F12 C22 F11 107.4(4) . . ?
F10 C22 C21 112.4(3) . . ?
F12 C22 C21 113.7(4) . . ?
F11 C22 C21 110.2(3) . . ?
N1 C4 C3 108.6(3) . . ?
N1 C4 C1 107.4(3) . . ?
C3 C4 C1 111.5(4) . . ?
N1 C4 C2 108.3(3) . . ?
C3 C4 C2 111.9(4) . . ?
C1 C4 C2 108.9(4) . . ?
F9 C18 F8 111.2(5) . . ?
F9 C18 F7 105.6(5) . . ?
F8 C18 F7 103.1(5) . . ?
F9 C18 C19 114.3(4) . . ?
F8 C18 C19 109.9(4) . . ?
F7 C18 C19 112.3(4) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O5 2.046(2) . ?
Co1 O2 2.060(2) . ?
Co1 O4 2.090(2) . ?
Co1 O1 2.091(2) . ?
Co1 O3 2.093(2) . ?
Co1 N4 2.109(3) 2_666 ?
O2 C14 1.259(4) . ?
O1 N1 1.295(3) . ?
N4 C11 1.313(4) . ?
N4 C12 1.360(4) . ?
N4 Co1 2.109(3) 2_666 ?
O4 C19 1.241(4) . ?
O3 C16 1.239(4) . ?
O5 C21 1.247(4) . ?
N1 C5 1.411(4) . ?
N1 C4 1.519(4) . ?
C14 C15 1.383(5) . ?
C14 C13 1.522(5) . ?
N2 C11 1.329(4) . ?
N2 N3 1.368(4) . ?
N2 C8 1.428(4) . ?
C21 C20 1.377(5) . ?
C21 C22 1.531(5) . ?
C5 C10 1.388(5) . ?
C5 C6 1.396(5) . ?
C12 N3 1.307(5) . ?
C8 C7 1.375(5) . ?
C8 C9 1.385(4) . ?
C16 C15 1.389(5) . ?
C16 C17 1.539(5) . ?
C9 C10 1.373(5) . ?
C19 C20 1.388(5) . ?
C19 C18 1.530(5) . ?
F2 C13 1.313(4) . ?
C13 F1 1.300(5) . ?
C13 F3 1.323(5) . ?
C17 F4 1.271(5) . ?
C17 F6 1.274(5) . ?
C17 F5 1.357(5) . ?
F10 C22 1.294(5) . ?
C6 C7 1.384(5) . ?
F11 C22 1.320(5) . ?
C22 F12 1.294(6) . ?
F9 C18 1.266(6) . ?
C4 C3 1.520(6) . ?
C4 C1 1.521(6) . ?
C4 C2 1.537(7) . ?
F8 C18 1.306(6) . ?
F7 C18 1.310(6) . ?
