#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/25/4312538.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_4312538
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        UMASS
_chemical_formula_moiety         'C22 H17 F12 Mn N4 O5 '
_chemical_formula_sum            'C22 H17 F12 Mn N4 O5'
_chemical_formula_weight         700.315
_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                93.1757(12)
_cell_angle_beta                 91.2499(12)
_cell_angle_gamma                114.458(2)
_cell_formula_units_Z            2
_cell_length_a                   9.7111(2)
_cell_length_b                   10.6775(3)
_cell_length_c                   14.7440(6)
_cell_measurement_reflns_used    4610
_cell_measurement_temperature    298
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      4.076
_cell_volume                     1387.80(8)
_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 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device       KappaCCD
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_UB_11      0.10659
_diffrn_orient_matrix_UB_12      -0.03827
_diffrn_orient_matrix_UB_13      0.00140
_diffrn_orient_matrix_UB_21      0.07209
_diffrn_orient_matrix_UB_22      0.07367
_diffrn_orient_matrix_UB_23      -0.00391
_diffrn_orient_matrix_UB_31      0.00472
_diffrn_orient_matrix_UB_32      0.00571
_diffrn_orient_matrix_UB_33      0.06761
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           ' MoK\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0299
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_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            8274
_diffrn_reflns_theta_full        25.09
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         4.16
_exptl_absorpt_coefficient_mu    0.597
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            RED-BROWN
_exptl_crystal_density_diffrn    1.676
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       NEEDLE
_exptl_crystal_F_000             700
_exptl_crystal_size_max          1.300
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.993
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.366
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         4874
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.366
_refine_ls_R_factor_all          0.0927
_refine_ls_R_factor_gt           0.0692
_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)+ (0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1900
_refine_ls_wR_factor_ref         0.2027
_reflns_number_gt                3700
_reflns_number_total             4874
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0349050si20030730_014852_2.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_cell_volume        1387.80(7)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C22 H17 F12 Mn N4 O5 '
_cod_database_code               4312538
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
Mn1 Mn 0.11307(6) 0.59860(6) 0.22808(4) 0.0465(3) Uani 1 1 d . . .
O5 O 0.0986(3) 0.6828(3) 0.0995(2) 0.0553(7) Uani 1 1 d . . .
O1 O 0.3415(3) 0.7496(3) 0.25677(19) 0.0507(7) Uani 1 1 d . . .
O3 O -0.1254(3) 0.4577(3) 0.2254(2) 0.0584(8) Uani 1 1 d . . .
O2 O 0.1206(3) 0.4963(3) 0.3473(2) 0.0567(7) Uani 1 1 d . . .
N2 N 0.7291(4) 0.6381(4) -0.0416(2) 0.0483(8) Uani 1 1 d . . .
O4 O 0.0629(3) 0.7674(3) 0.2794(2) 0.0545(7) Uani 1 1 d . . .
C3 C 0.6699(4) 0.6684(4) 0.0406(3) 0.0469(9) Uani 1 1 d . . .
N3 N 0.8137(4) 0.5434(4) -0.1477(3) 0.0518(8) Uani 1 1 d . . .
N1 N 0.4656(4) 0.7353(4) 0.2738(2) 0.0506(8) Uani 1 1 d . . .
C19 C 0.1039(5) 0.8794(5) 0.2449(3) 0.0537(10) Uani 1 1 d . . .
C6 C 0.5423(4) 0.7160(4) 0.1972(3) 0.0458(9) Uani 1 1 d . . .
C15 C -0.1254(5) 0.3162(5) 0.3431(3) 0.0615(12) Uani 1 1 d . . .
F1 F 0.1861(5) 0.3022(4) 0.4354(2) 0.1011(12) Uani 1 1 d . . .
C2 C 0.7833(5) 0.5448(4) -0.0614(3) 0.0528(10) Uani 1 1 d . . .
C14 C 0.0214(5) 0.3901(5) 0.3760(3) 0.0503(10) Uani 1 1 d . . .
C21 C 0.1324(5) 0.8078(5) 0.0899(3) 0.0511(10) Uani 1 1 d . . .
C7 C 0.5143(5) 0.7604(5) 0.1147(3) 0.0524(10) Uani 1 1 d . . .
N4 N 0.7239(5) 0.7029(4) -0.1181(3) 0.0625(10) Uani 1 1 d . . .
C8 C 0.5769(5) 0.7375(4) 0.0372(3) 0.0522(10) Uani 1 1 d . . .
C1 C 0.7740(5) 0.6413(5) -0.1796(3) 0.0628(12) Uani 1 1 d . . .
C22 C 0.1740(6) 0.8526(5) -0.0053(3) 0.0658(12) Uani 1 1 d . . .
C16 C -0.1877(5) 0.3591(5) 0.2726(3) 0.0543(10) Uani 1 1 d . . .
C18 C 0.1216(6) 1.0031(5) 0.3096(4) 0.0660(13) Uani 1 1 d . . .
C20 C 0.1373(6) 0.9076(5) 0.1548(3) 0.0611(12) Uani 1 1 d . . .
F8 F 0.0320(6) 1.0623(5) 0.2808(3) 0.1263(15) Uani 1 1 d . . .
C13 C 0.0767(6) 0.3378(6) 0.4582(3) 0.0700(13) Uani 1 1 d . . .
F11 F 0.3193(4) 0.9234(5) -0.0104(3) 0.1149(14) Uani 1 1 d . . .
F7 F 0.0700(6) 0.9693(4) 0.3882(3) 0.1286(16) Uani 1 1 d . . .
F2 F 0.1386(6) 0.4355(5) 0.5231(2) 0.1181(15) Uani 1 1 d . . .
C4 C 0.7030(5) 0.6285(6) 0.1223(3) 0.0686(14) Uani 1 1 d . . .
F10 F 0.1335(6) 0.7534(5) -0.0667(3) 0.152(2) Uani 1 1 d . . .
C9 C 0.5262(5) 0.7630(6) 0.3715(3) 0.0655(13) Uani 1 1 d . . .
F9 F 0.2506(5) 1.1010(5) 0.3109(4) 0.158(2) Uani 1 1 d . . .
C5 C 0.6410(5) 0.6511(6) 0.2002(3) 0.0655(13) Uani 1 1 d . . .
F12 F 0.1166(7) 0.9368(7) -0.0325(3) 0.171(3) Uani 1 1 d . . .
F3 F -0.0276(6) 0.2310(6) 0.4913(4) 0.175(3) Uani 1 1 d . . .
F5 F -0.4354(4) 0.3247(7) 0.3014(5) 0.185(3) Uani 1 1 d . . .
C11 C 0.5049(7) 0.6242(7) 0.4093(4) 0.0909(18) Uani 1 1 d . . .
C17 C -0.3577(6) 0.2747(7) 0.2500(5) 0.0865(18) Uani 1 1 d . . .
C10 C 0.4332(8) 0.8217(8) 0.4250(4) 0.103(2) Uani 1 1 d . . .
C12 C 0.6930(6) 0.8620(8) 0.3748(5) 0.110(2) Uani 1 1 d . . .
F6 F -0.3988(4) 0.2883(6) 0.1689(4) 0.151(2) Uani 1 1 d . . .
F4 F -0.4045(5) 0.1475(5) 0.2580(6) 0.204(3) Uani 1 1 d . . .
H15 H -0.1846 0.2350 0.3693 0.074 Uiso 1 1 d R . .
H2 H 0.7977 0.4884 -0.0198 0.063 Uiso 1 1 d R . .
H7 H 0.4519 0.8069 0.1124 0.063 Uiso 1 1 d R . .
H8 H 0.5573 0.7679 -0.0175 0.063 Uiso 1 1 d R . .
H1 H 0.7821 0.6629 -0.2400 0.075 Uiso 1 1 d R . .
H20 H 0.1643 0.9970 0.1379 0.073 Uiso 1 1 d R . .
H4 H 0.7687 0.5853 0.1246 0.082 Uiso 1 1 d R . .
H5 H 0.6643 0.6237 0.2551 0.079 Uiso 1 1 d R . .
H11A H 0.3991 0.5638 0.4070 0.109 Uiso 1 1 d R . .
H11B H 0.5579 0.5826 0.3732 0.109 Uiso 1 1 d R . .
H11C H 0.5445 0.6401 0.4711 0.109 Uiso 1 1 d R . .
H10A H 0.3292 0.7560 0.4219 0.124 Uiso 1 1 d R . .
H10B H 0.4708 0.8414 0.4873 0.124 Uiso 1 1 d R . .
H10C H 0.4407 0.9051 0.3997 0.124 Uiso 1 1 d R . .
H12A H 0.7489 0.8202 0.3417 0.132 Uiso 1 1 d R . .
H12B H 0.7036 0.9451 0.3478 0.132 Uiso 1 1 d R . .
H12C H 0.7315 0.8836 0.4369 0.132 Uiso 1 1 d 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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 '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'
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
O2 Mn1 O1 91.47(11) . . ?
O2 Mn1 O4 103.29(12) . . ?
O1 Mn1 O4 81.65(11) . . ?
O2 Mn1 O5 174.32(12) . . ?
O1 Mn1 O5 91.90(12) . . ?
O4 Mn1 O5 81.72(11) . . ?
O2 Mn1 O3 82.12(11) . . ?
O1 Mn1 O3 168.94(12) . . ?
O4 Mn1 O3 91.01(11) . . ?
O5 Mn1 O3 95.24(11) . . ?
O2 Mn1 N3 89.52(13) . 2_665 ?
O1 Mn1 N3 93.08(11) . 2_665 ?
O4 Mn1 N3 166.20(13) . 2_665 ?
O5 Mn1 N3 85.74(12) . 2_665 ?
O3 Mn1 N3 95.85(12) . 2_665 ?
C21 O5 Mn1 124.5(3) . . ?
N1 O1 Mn1 130.9(2) . . ?
C16 O3 Mn1 128.1(3) . . ?
C14 O2 Mn1 129.1(3) . . ?
C2 N2 N4 109.2(3) . . ?
C2 N2 C3 130.5(4) . . ?
N4 N2 C3 120.2(3) . . ?
C19 O4 Mn1 124.5(3) . . ?
C4 C3 C8 119.9(4) . . ?
C4 C3 N2 120.8(3) . . ?
C8 C3 N2 119.3(4) . . ?
C2 N3 C1 103.1(4) . . ?
C2 N3 Mn1 129.4(3) . 2_665 ?
C1 N3 Mn1 127.2(3) . 2_665 ?
O1 N1 C6 116.3(3) . . ?
O1 N1 C9 116.7(3) . . ?
C6 N1 C9 126.2(3) . . ?
O4 C19 C20 128.2(4) . . ?
O4 C19 C18 115.9(4) . . ?
C20 C19 C18 115.9(4) . . ?
C7 C6 C5 118.6(4) . . ?
C7 C6 N1 118.3(3) . . ?
C5 C6 N1 123.1(4) . . ?
C14 C15 C16 122.0(4) . . ?
N3 C2 N2 110.6(4) . . ?
O2 C14 C15 128.6(4) . . ?
O2 C14 C13 113.6(4) . . ?
C15 C14 C13 117.8(4) . . ?
O5 C21 C20 128.0(4) . . ?
O5 C21 C22 114.9(4) . . ?
C20 C21 C22 117.1(4) . . ?
C8 C7 C6 121.4(4) . . ?
C1 N4 N2 102.7(3) . . ?
C7 C8 C3 119.3(4) . . ?
N4 C1 N3 114.4(4) . . ?
F10 C22 F11 107.0(5) . . ?
F10 C22 F12 105.9(5) . . ?
F11 C22 F12 103.3(5) . . ?
F10 C22 C21 114.3(4) . . ?
F11 C22 C21 111.9(4) . . ?
F12 C22 C21 113.5(5) . . ?
O3 C16 C15 128.8(4) . . ?
O3 C16 C17 115.1(4) . . ?
C15 C16 C17 116.1(5) . . ?
F9 C18 F7 114.8(6) . . ?
F9 C18 F8 102.1(5) . . ?
F7 C18 F8 100.4(4) . . ?
F9 C18 C19 113.7(4) . . ?
F7 C18 C19 113.5(4) . . ?
F8 C18 C19 110.7(5) . . ?
C21 C20 C19 122.4(4) . . ?
F3 C13 F2 109.4(5) . . ?
F3 C13 F1 106.8(5) . . ?
F2 C13 F1 104.2(5) . . ?
F3 C13 C14 114.1(5) . . ?
F2 C13 C14 111.6(4) . . ?
F1 C13 C14 110.2(4) . . ?
C5 C4 C3 121.1(4) . . ?
C10 C9 N1 108.0(4) . . ?
C10 C9 C12 112.1(5) . . ?
N1 C9 C12 108.9(4) . . ?
C10 C9 C11 108.6(5) . . ?
N1 C9 C11 108.4(4) . . ?
C12 C9 C11 110.9(5) . . ?
C4 C5 C6 119.6(4) . . ?
F4 C17 F6 106.4(7) . . ?
F4 C17 F5 109.5(7) . . ?
F6 C17 F5 102.8(6) . . ?
F4 C17 C16 115.1(5) . . ?
F6 C17 C16 113.0(5) . . ?
F5 C17 C16 109.2(5) . . ?
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
Mn1 O2 2.136(3) . ?
Mn1 O1 2.150(3) . ?
Mn1 O4 2.156(3) . ?
Mn1 O5 2.168(3) . ?
Mn1 O3 2.175(3) . ?
Mn1 N3 2.222(3) 2_665 ?
O5 C21 1.253(5) . ?
O1 N1 1.297(4) . ?
O3 C16 1.237(5) . ?
O2 C14 1.248(5) . ?
N2 C2 1.327(5) . ?
N2 N4 1.367(5) . ?
N2 C3 1.430(5) . ?
O4 C19 1.237(5) . ?
C3 C4 1.375(6) . ?
C3 C8 1.384(5) . ?
N3 C2 1.313(6) . ?
N3 C1 1.357(6) . ?
N3 Mn1 2.222(3) 2_665 ?
N1 C6 1.417(5) . ?
N1 C9 1.511(6) . ?
C19 C20 1.394(7) . ?
C19 C18 1.532(7) . ?
C6 C7 1.390(6) . ?
C6 C5 1.398(6) . ?
C15 C14 1.373(6) . ?
C15 C16 1.383(6) . ?
F1 C13 1.313(6) . ?
C14 C13 1.538(6) . ?
C21 C20 1.377(7) . ?
C21 C22 1.517(7) . ?
C7 C8 1.363(6) . ?
N4 C1 1.307(6) . ?
C22 F10 1.276(6) . ?
C22 F11 1.303(6) . ?
C22 F12 1.314(6) . ?
C16 C17 1.537(7) . ?
C18 F9 1.255(6) . ?
C18 F7 1.283(6) . ?
C18 F8 1.344(6) . ?
C13 F3 1.300(7) . ?
C13 F2 1.307(7) . ?
C4 C5 1.363(7) . ?
C9 C10 1.507(8) . ?
C9 C12 1.522(7) . ?
C9 C11 1.546(8) . ?
F5 C17 1.319(8) . ?
C17 F4 1.254(7) . ?
C17 F6 1.287(8) . ?
