#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/25/4312541.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_4312541
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        'Lahti group'
_chemical_formula_moiety         'C22 H17 F12 N4 Ni O5 '
_chemical_formula_sum            'C22 H17 F12 N4 Ni O5'
_chemical_formula_weight         704.087
_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                93.1995(7)
_cell_angle_beta                 92.5002(8)
_cell_angle_gamma                116.6025(8)
_cell_formula_units_Z            2
_cell_length_a                   9.8155(2)
_cell_length_b                   10.5185(2)
_cell_length_c                   15.0198(3)
_cell_measurement_reflns_used    4501
_cell_measurement_temperature    298
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      4.076
_cell_volume                     1380.29(5)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device       KappaCCD
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_UB_11      -0.09725
_diffrn_orient_matrix_UB_12      -0.06002
_diffrn_orient_matrix_UB_13      0.00102
_diffrn_orient_matrix_UB_21      -0.04402
_diffrn_orient_matrix_UB_22      -0.02200
_diffrn_orient_matrix_UB_23      -0.09468
_diffrn_orient_matrix_UB_31      0.03041
_diffrn_orient_matrix_UB_32      -0.05918
_diffrn_orient_matrix_UB_33      -0.00675
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           ' MoK\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0207
_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            8751
_diffrn_reflns_theta_full        25.07
_diffrn_reflns_theta_max         25.07
_diffrn_reflns_theta_min         4.09
_exptl_absorpt_coefficient_mu    0.825
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            GREEN
_exptl_crystal_density_diffrn    1.694
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       NEEDLE
_exptl_crystal_F_000             706
_exptl_crystal_size_max          1.000
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.254
_refine_diff_density_min         -0.140
_refine_diff_density_rms         0.018
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         4819
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_gt           0.0492
_refine_ls_shift/su_max          0.120
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0679P)²+0.1392P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1315
_refine_ls_wR_factor_ref         0.1375
_reflns_number_gt                4320
_reflns_number_total             4819
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0349050si20030730_014852_5.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 F12 N4 Ni O5 '
_cod_database_code               4312541
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
Ni1 Ni 0.86200(4) 0.39763(4) 0.27566(3) 0.0595(8) Uani 1 1 d . . .
O5 O 0.8770(3) 0.3157(2) 0.39269(15) 0.0667(9) Uani 1 1 d . . .
O1 O 0.3644(2) 0.7574(2) 0.74418(16) 0.0667(9) Uani 1 1 d . . .
O4 O 0.8985(3) 0.2412(2) 0.21060(16) 0.0690(10) Uani 1 1 d . . .
N4 N 0.8070(3) 0.5393(3) 0.34594(18) 0.0623(10) Uani 1 1 d . . .
O3 O 1.0927(3) 0.5318(2) 0.29020(16) 0.0699(10) Uani 1 1 d . . .
O2 O 0.8484(3) 0.4818(3) 0.16032(16) 0.0710(10) Uani 1 1 d . . .
C5 C 0.5568(3) 0.7187(3) 0.6859(2) 0.0632(11) Uani 1 1 d . . .
N2 N 0.7326(3) 0.6389(3) 0.45100(18) 0.0609(10) Uani 1 1 d . . .
N3 N 0.7252(4) 0.7037(3) 0.3760(2) 0.0759(11) Uani 1 1 d . . .
C11 C 0.7812(4) 0.5420(3) 0.4310(2) 0.0627(10) Uani 1 1 d . . .
N1 N 0.4855(3) 0.7408(3) 0.76122(19) 0.0674(10) Uani 1 1 d . . .
F11 F 0.6773(3) 0.0692(3) 0.50084(18) 0.1024(11) Uani 1 1 d . . .
C12 C 0.7709(4) 0.6407(4) 0.3155(2) 0.0738(12) Uani 1 1 d . . .
C9 C 0.5848(4) 0.7363(3) 0.5283(2) 0.0655(11) Uani 1 1 d . . .
C21 C 0.8537(3) 0.1891(3) 0.3979(2) 0.0629(11) Uani 1 1 d . . .
F12 F 0.8824(4) 0.2431(3) 0.55449(17) 0.1185(13) Uani 1 1 d . . .
C19 C 0.8680(4) 0.1256(3) 0.2421(2) 0.0670(11) Uani 1 1 d . . .
C10 C 0.5255(4) 0.7609(3) 0.6046(2) 0.0661(11) Uani 1 1 d . . .
C16 C 1.1604(4) 0.6290(4) 0.2414(2) 0.0714(11) Uani 1 1 d . . .
F7 F 0.9076(5) 0.0452(3) 0.10002(19) 0.1306(14) Uani 1 1 d . . .
C8 C 0.6779(3) 0.6695(3) 0.5319(2) 0.0606(10) Uani 1 1 d . . .
C14 C 0.9545(4) 0.5859(4) 0.1306(2) 0.0701(11) Uani 1 1 d . . .
C6 C 0.6539(4) 0.6540(4) 0.6887(2) 0.0751(12) Uani 1 1 d . . .
C20 C 0.8459(4) 0.0914(4) 0.3303(2) 0.0737(12) Uani 1 1 d . . .
C15 C 1.1021(5) 0.6630(4) 0.1658(3) 0.0824(13) Uani 1 1 d . . .
F2 F 0.8193(5) 0.6925(4) 0.0617(2) 0.1510(17) Uani 1 1 d . . .
C22 C 0.8245(4) 0.1383(4) 0.4918(2) 0.0728(12) Uani 1 1 d . . .
C7 C 0.7148(4) 0.6309(4) 0.6119(2) 0.0742(12) Uani 1 1 d . . .
F10 F 0.8800(4) 0.0481(4) 0.5097(2) 0.1289(13) Uani 1 1 d . . .
F1 F 0.8232(5) 0.5242(4) -0.01234(18) 0.1428(15) Uani 1 1 d . . .
C4 C 0.5527(5) 0.7704(5) 0.8576(3) 0.0860(13) Uani 1 1 d . . .
F8 F 0.9266(5) -0.0660(3) 0.2039(2) 0.1330(14) Uani 1 1 d . . .
F4 F 1.3785(4) 0.8514(4) 0.2619(4) 0.201(3) Uani 1 1 d . . .
C18 C 0.8501(5) 0.0041(4) 0.1738(3) 0.0835(13) Uani 1 1 d . . .
F9 F 0.7132(4) -0.0938(4) 0.1629(3) 0.186(2) Uani 1 1 d . . .
C13 C 0.9069(6) 0.6317(5) 0.0446(3) 0.0948(14) Uani 1 1 d . . .
F5 F 1.4112(4) 0.6723(6) 0.2204(4) 0.194(2) Uani 1 1 d . . .
F3 F 1.0197(6) 0.7164(7) 0.0031(3) 0.226(3) Uani 1 1 d . . .
C1 C 0.4680(6) 0.8352(6) 0.9110(3) 0.1119(18) Uani 1 1 d . . .
F6 F 1.3709(4) 0.7053(4) 0.3493(3) 0.1535(17) Uani 1 1 d . . .
C3 C 0.7210(5) 0.8765(7) 0.8587(4) 0.124(2) Uani 1 1 d . . .
C17 C 1.3309(5) 0.7187(5) 0.2670(4) 0.0983(15) Uani 1 1 d . . .
C2 C 0.5284(6) 0.6285(7) 0.8938(3) 0.1116(18) Uani 1 1 d . . .
H11 H 0.7949 0.4843 0.4715 0.075 Uiso 1 1 calc R . .
H12 H 0.7783 0.6633 0.2563 0.089 Uiso 1 1 calc R . .
H9 H 0.5624 0.7646 0.4743 0.079 Uiso 1 1 calc R . .
H10 H 0.4634 0.8064 0.6019 0.079 Uiso 1 1 calc R . .
H6 H 0.6776 0.6263 0.7426 0.090 Uiso 1 1 calc R . .
H20 H 0.8252 -0.0003 0.3440 0.088 Uiso 1 1 calc R . .
H15 H 1.1665 0.7423 0.1376 0.099 Uiso 1 1 calc R . .
H7 H 0.7806 0.5893 0.6142 0.089 Uiso 1 1 calc R . .
H1A H 0.3619 0.7679 0.9093 0.168 Uiso 1 1 calc R . .
H1B H 0.4777 0.9203 0.8856 0.168 Uiso 1 1 calc R . .
H1C H 0.5107 0.8583 0.9719 0.168 Uiso 1 1 calc R . .
H3A H 0.7735 0.8344 0.8249 0.186 Uiso 1 1 calc R . .
H3B H 0.7651 0.9010 0.9193 0.186 Uiso 1 1 calc R . .
H3C H 0.7305 0.9610 0.8325 0.186 Uiso 1 1 calc R . .
H2A H 0.5827 0.5883 0.8599 0.167 Uiso 1 1 calc R . .
H2B H 0.4214 0.5634 0.8884 0.167 Uiso 1 1 calc R . .
H2C H 0.5661 0.6452 0.9555 0.167 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'
Ni Ni 0.3393 1.1124 '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 Ni1 O5 179.17(9) . . ?
O2 Ni1 O4 91.98(9) . . ?
O5 Ni1 O4 88.73(9) . . ?
O2 Ni1 N4 91.06(10) . . ?
O5 Ni1 N4 88.27(10) . . ?
O4 Ni1 N4 174.37(9) . . ?
O2 Ni1 O3 89.26(10) . . ?
O5 Ni1 O3 90.29(9) . . ?
O4 Ni1 O3 91.28(9) . . ?
N4 Ni1 O3 93.50(10) . . ?
O2 Ni1 O1 92.19(10) . 2_666 ?
O5 Ni1 O1 88.35(9) . 2_666 ?
O4 Ni1 O1 81.92(9) . 2_666 ?
N4 Ni1 O1 93.23(9) . 2_666 ?
O3 Ni1 O1 173.09(9) . 2_666 ?
C21 O5 Ni1 123.5(2) . . ?
N1 O1 Ni1 128.55(19) . 2_666 ?
C19 O4 Ni1 122.5(2) . . ?
C11 N4 C12 102.9(3) . . ?
C11 N4 Ni1 127.4(2) . . ?
C12 N4 Ni1 129.4(2) . . ?
C16 O3 Ni1 124.4(2) . . ?
C14 O2 Ni1 125.5(2) . . ?
C10 C5 C6 118.5(3) . . ?
C10 C5 N1 118.1(3) . . ?
C6 C5 N1 123.4(3) . . ?
C11 N2 N3 109.3(3) . . ?
C11 N2 C8 130.0(3) . . ?
N3 N2 C8 120.4(2) . . ?
C12 N3 N2 102.8(3) . . ?
N4 C11 N2 110.5(3) . . ?
O1 N1 C5 116.0(3) . . ?
O1 N1 C4 117.7(3) . . ?
C5 N1 C4 125.5(3) . . ?
N3 C12 N4 114.6(3) . . ?
C10 C9 C8 119.8(3) . . ?
O5 C21 C20 128.4(3) . . ?
O5 C21 C22 114.2(3) . . ?
C20 C21 C22 117.4(3) . . ?
O4 C19 C20 128.8(3) . . ?
O4 C19 C18 115.1(3) . . ?
C20 C19 C18 116.0(3) . . ?
C9 C10 C5 121.0(3) . . ?
O3 C16 C15 128.4(3) . . ?
O3 C16 C17 115.3(3) . . ?
C15 C16 C17 116.3(4) . . ?
C7 C8 C9 120.5(3) . . ?
C7 C8 N2 120.6(3) . . ?
C9 C8 N2 118.9(3) . . ?
O2 C14 C15 128.5(3) . . ?
O2 C14 C13 113.6(3) . . ?
C15 C14 C13 117.9(4) . . ?
C7 C6 C5 120.3(3) . . ?
C21 C20 C19 122.1(3) . . ?
C14 C15 C16 123.3(3) . . ?
F12 C22 F11 107.3(3) . . ?
F12 C22 F10 107.1(3) . . ?
F11 C22 F10 105.6(3) . . ?
F12 C22 C21 112.7(3) . . ?
F11 C22 C21 110.6(3) . . ?
F10 C22 C21 113.0(3) . . ?
C8 C7 C6 119.9(3) . . ?
C1 C4 N1 107.7(3) . . ?
C1 C4 C3 110.2(4) . . ?
N1 C4 C3 107.7(4) . . ?
C1 C4 C2 109.9(4) . . ?
N1 C4 C2 108.7(3) . . ?
C3 C4 C2 112.6(4) . . ?
F9 C18 F7 112.6(4) . . ?
F9 C18 F8 102.5(4) . . ?
F7 C18 F8 102.9(4) . . ?
F9 C18 C19 112.3(3) . . ?
F7 C18 C19 114.3(3) . . ?
F8 C18 C19 111.2(4) . . ?
F3 C13 F1 106.5(5) . . ?
F3 C13 F2 108.8(5) . . ?
F1 C13 F2 104.1(4) . . ?
F3 C13 C14 113.9(4) . . ?
F1 C13 C14 112.6(4) . . ?
F2 C13 C14 110.3(4) . . ?
F4 C17 F5 110.6(5) . . ?
F4 C17 F6 105.5(5) . . ?
F5 C17 F6 101.8(5) . . ?
F4 C17 C16 114.4(4) . . ?
F5 C17 C16 110.8(4) . . ?
F6 C17 C16 112.9(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
Ni1 O2 2.015(2) . ?
Ni1 O5 2.028(2) . ?
Ni1 O4 2.042(2) . ?
Ni1 N4 2.054(3) . ?
Ni1 O3 2.056(2) . ?
Ni1 O1 2.081(2) 2_666 ?
O5 C21 1.254(4) . ?
O1 N1 1.294(3) . ?
O1 Ni1 2.081(2) 2_666 ?
O4 C19 1.242(4) . ?
N4 C11 1.315(4) . ?
N4 C12 1.361(4) . ?
O3 C16 1.241(4) . ?
O2 C14 1.248(4) . ?
C5 C10 1.389(5) . ?
C5 C6 1.398(5) . ?
C5 N1 1.418(4) . ?
N2 C11 1.330(4) . ?
N2 N3 1.365(4) . ?
N2 C8 1.428(4) . ?
N3 C12 1.304(5) . ?
N1 C4 1.520(5) . ?
F11 C22 1.312(4) . ?
C9 C10 1.370(5) . ?
C9 C8 1.381(4) . ?
C21 C20 1.379(5) . ?
C21 C22 1.529(5) . ?
F12 C22 1.304(4) . ?
C19 C20 1.393(5) . ?
C19 C18 1.534(5) . ?
C16 C15 1.385(5) . ?
C16 C17 1.526(6) . ?
F7 C18 1.275(5) . ?
C8 C7 1.373(5) . ?
C14 C15 1.368(6) . ?
C14 C13 1.529(5) . ?
C6 C7 1.381(5) . ?
F2 C13 1.307(6) . ?
C22 F10 1.321(4) . ?
F1 C13 1.297(6) . ?
C4 C1 1.518(6) . ?
C4 C3 1.523(6) . ?
C4 C2 1.538(7) . ?
F8 C18 1.348(5) . ?
F4 C17 1.266(6) . ?
C18 F9 1.271(5) . ?
C13 F3 1.284(6) . ?
F5 C17 1.305(6) . ?
F6 C17 1.316(6) . ?
