#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:45:23 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179261 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/81/4318199.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_4318199
loop_
_publ_author_name
'Mohammed Fettouhi'
'Bassam El Ali'
'Abdel Moneim El-Ghanam'
'Stéphane Golhen'
'Lahcène Ouahab'
'Nathalie Daro'
'Jean-Pascal Sutter'
_publ_contact_author_address
;
LCSIM - UMR 6511 CNRS Universite de Rennes 1
Batiment 10B
Avenue du General Leclerc
35042 Rennes cedex
France
;
_publ_contact_author_email       Ouahab@univ-rennes1.fr
_publ_contact_author_name        'Dr OUAHAB Lahcene'
_publ_section_title
;
 Temperature Dependence of the Crystal Lattice Organization of
 Coordination Compounds Involving Nitronyl Nitroxide Radicals: A Magnetic
 and Structural Investigation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3705
_journal_page_last               3712
_journal_paper_doi               10.1021/ic020021p
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C50 H64 Cd N14 O4 S2'
_chemical_formula_weight         1101.67
_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                91.3115(13)
_cell_angle_beta                 99.581(9)
_cell_angle_gamma                97.721(19)
_cell_formula_units_Z            1
_cell_length_a                   7.3016(12)
_cell_length_b                   13.744(3)
_cell_length_c                   14.2278(12)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      10.596
_cell_measurement_theta_min      4.494
_cell_volume                     1393.6(4)
_computing_cell_refinement       MolEN
_computing_data_collection       'Enraf Nonius CAD4'
_computing_data_reduction        MolEN
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       θ-2θ
_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  0.0218
_diffrn_reflns_av_sigmaI/netI    0.0489
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5888
_diffrn_reflns_theta_full        25.97
_diffrn_reflns_theta_max         25.97
_diffrn_reflns_theta_min         1.45
_diffrn_standards_interval_count 250
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.521
_exptl_absorpt_correction_T_max  0.999779
_exptl_absorpt_correction_T_min  0.923326
_exptl_absorpt_correction_type   \y-scan
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             578
_refine_diff_density_max         2.115
_refine_diff_density_min         -0.813
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         5432
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0856
_refine_ls_R_factor_gt           0.0601
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1099P)²+1.4319P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1626
_refine_ls_wR_factor_ref         0.1781
_reflns_number_gt                4505
_reflns_number_total             5432
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020021p_2.cif
_cod_data_source_block           A
_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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1099P)^2^+1.4319P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1099P)^2^+1.4319P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4318199
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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 0.0000 0.0000 0.0000 0.03421(18) Uani 1 d S . .
N1 N 0.1110(5) -0.1508(3) 0.0438(3) 0.0421(9) Uani 1 d . . .
N2 N 0.5028(6) -0.4320(3) 0.1359(3) 0.0501(10) Uani 1 d . . .
N3 N 0.2452(7) -0.4666(3) 0.2000(4) 0.0567(12) Uani 1 d . . .
O1 O 0.6172(6) -0.3895(3) 0.0859(4) 0.0756(13) Uani 1 d . . .
C1 C 0.0032(7) -0.2283(4) 0.0675(5) 0.0550(14) Uani 1 d . . .
H1 H -0.1248 -0.2257 0.0620 0.066 Uiso 1 calc R . .
C2 C 0.0704(7) -0.3125(4) 0.0998(5) 0.0548(14) Uani 1 d . . .
H2 H -0.0113 -0.3652 0.1153 0.066 Uiso 1 calc R . .
C3 C 0.2582(7) -0.3183(3) 0.1088(4) 0.0403(10) Uani 1 d . . .
C4 C 0.3713(8) -0.2375(4) 0.0840(5) 0.0617(16) Uani 1 d . . .
H4 H 0.4996 -0.2381 0.0880 0.074 Uiso 1 calc R . .
C5 C 0.2917(8) -0.1568(4) 0.0534(5) 0.0605(16) Uani 1 d . . .
H5 H 0.3703 -0.1026 0.0383 0.073 Uiso 1 calc R . .
C6 C 0.3323(7) -0.4057(3) 0.1479(4) 0.0443(11) Uani 1 d . . .
C7 C 0.5511(9) -0.5112(4) 0.2005(4) 0.0574(14) Uani 1 d . . .
C8 C 0.3523(9) -0.5515(4) 0.2191(4) 0.0585(14) Uani 1 d . . .
C9 C 0.6835(12) -0.4603(6) 0.2864(6) 0.088(2) Uani 1 d . . .
H9A H 0.8027 -0.4378 0.2686 0.132 Uiso 1 calc R . .
H9B H 0.7000 -0.5057 0.3364 0.132 Uiso 1 calc R . .
H9C H 0.6316 -0.4052 0.3086 0.132 Uiso 1 calc R . .
C10 C 0.6504(11) -0.5832(5) 0.1516(6) 0.082(2) Uani 1 d . . .
H10A H 0.5665 -0.6150 0.0971 0.123 Uiso 1 calc R . .
H10B H 0.6886 -0.6316 0.1955 0.123 Uiso 1 calc R . .
H10C H 0.7589 -0.5482 0.1313 0.123 Uiso 1 calc R . .
C11 C 0.2518(11) -0.6330(4) 0.1481(6) 0.0752(19) Uani 1 d . . .
H11A H 0.2558 -0.6123 0.0844 0.113 Uiso 1 calc R . .
H11B H 0.1236 -0.6478 0.1568 0.113 Uiso 1 calc R . .
H11C H 0.3124 -0.6907 0.1581 0.113 Uiso 1 calc R . .
C12 C 0.3448(14) -0.5829(6) 0.3207(5) 0.090(2) Uani 1 d . . .
H12A H 0.4083 -0.5307 0.3651 0.135 Uiso 1 calc R . .
H12B H 0.4051 -0.6405 0.3317 0.135 Uiso 1 calc R . .
H12C H 0.2164 -0.5972 0.3291 0.135 Uiso 1 calc R . .
N4 N 0.2088(6) 0.0812(3) 0.1353(3) 0.0432(9) Uani 1 d . . .
N5 N 0.7764(7) 0.2150(4) 0.3962(3) 0.0630(13) Uani 1 d . . .
N6 N 0.5402(8) 0.1681(5) 0.4730(4) 0.0730(15) Uani 1 d . . .
O3 O 0.8642(8) 0.2371(6) 0.3279(3) 0.110(2) Uani 1 d . . .
C13 C 0.3909(7) 0.0981(5) 0.1362(4) 0.0554(14) Uani 1 d . . .
H13 H 0.4340 0.0865 0.0796 0.066 Uiso 1 calc R . .
C14 C 0.5218(7) 0.1317(5) 0.2153(4) 0.0556(14) Uani 1 d . . .
H14 H 0.6488 0.1431 0.2115 0.067 Uiso 1 calc R . .
C15 C 0.4617(7) 0.1478(4) 0.2994(3) 0.0444(11) Uani 1 d . . .
C16 C 0.2714(8) 0.1340(4) 0.2986(4) 0.0532(13) Uani 1 d . . .
H16 H 0.2243 0.1465 0.3539 0.064 Uiso 1 calc R . .
C17 C 0.1520(7) 0.1016(4) 0.2162(4) 0.0523(13) Uani 1 d . . .
H17 H 0.0237 0.0935 0.2170 0.063 Uiso 1 calc R . .
C18 C 0.5903(7) 0.1780(4) 0.3901(4) 0.0477(12) Uani 1 d . . .
C19 C 0.7068(10) 0.1988(6) 0.5485(5) 0.079(2) Uani 1 d . . .
C20 C 0.8618(10) 0.2381(9) 0.4976(5) 0.111(4) Uani 1 d . . .
C21 C 0.661(2) 0.2588(18) 0.6196(11) 0.299(15) Uani 1 d . . .
H21A H 0.5608 0.2240 0.6466 0.448 Uiso 1 calc R . .
H21B H 0.6225 0.3175 0.5922 0.448 Uiso 1 calc R . .
H21C H 0.7690 0.2759 0.6686 0.448 Uiso 1 calc R . .
C22 C 0.777(3) 0.0980(13) 0.574(2) 0.50(3) Uani 1 d . . .
H22A H 0.8022 0.0662 0.5181 0.747 Uiso 1 calc R . .
H22B H 0.6817 0.0567 0.5998 0.747 Uiso 1 calc R . .
H22C H 0.8893 0.1094 0.6213 0.747 Uiso 1 calc R . .
C23 C 1.0546(13) 0.2396(11) 0.5210(6) 0.140(5) Uani 1 d . . .
H23A H 1.1145 0.2717 0.4726 0.210 Uiso 1 calc R . .
H23B H 1.0829 0.1735 0.5254 0.210 Uiso 1 calc R . .
H23C H 1.0997 0.2748 0.5813 0.210 Uiso 1 calc R . .
C24 C 0.858(2) 0.3619(8) 0.5072(9) 0.184(7) Uani 1 d . . .
H24A H 0.7314 0.3753 0.4915 0.276 Uiso 1 calc R . .
H24B H 0.9321 0.3943 0.4642 0.276 Uiso 1 calc R . .
H24C H 0.9096 0.3857 0.5715 0.276 Uiso 1 calc R . .
S1 S 0.2664(4) 0.0951(3) -0.26765(17) 0.1281(12) Uani 1 d . . .
N7 N 0.2367(6) 0.0338(3) -0.0889(3) 0.0454(10) Uani 1 d . . .
C25 C 0.2466(7) 0.0601(4) -0.1612(4) 0.0535(13) Uani 1 d . . .
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
N7 Cd1 N7 180.0 2 . ?
N7 Cd1 N1 90.03(15) 2 . ?
N7 Cd1 N1 89.97(15) . . ?
N7 Cd1 N1 89.97(15) 2 2 ?
N7 Cd1 N1 90.03(15) . 2 ?
N1 Cd1 N1 180.0 . 2 ?
N7 Cd1 N4 91.48(14) 2 . ?
N7 Cd1 N4 88.52(14) . . ?
N1 Cd1 N4 89.15(14) . . ?
N1 Cd1 N4 90.85(14) 2 . ?
N7 Cd1 N4 88.52(14) 2 2 ?
N7 Cd1 N4 91.48(14) . 2 ?
N1 Cd1 N4 90.85(14) . 2 ?
N1 Cd1 N4 89.15(14) 2 2 ?
N4 Cd1 N4 180.0 . 2 ?
C5 N1 C1 116.5(4) . . ?
C5 N1 Cd1 119.7(3) . . ?
C1 N1 Cd1 123.6(3) . . ?
O1 N2 C6 127.1(4) . . ?
O1 N2 C7 122.5(4) . . ?
C6 N2 C7 110.0(4) . . ?
C6 N3 C8 108.8(5) . . ?
N1 C1 C2 123.4(5) . . ?
C3 C2 C1 119.6(5) . . ?
C2 C3 C4 117.1(4) . . ?
C2 C3 C6 120.0(4) . . ?
C4 C3 C6 122.9(4) . . ?
C5 C4 C3 118.9(5) . . ?
N1 C5 C4 124.4(5) . . ?
N3 C6 N2 112.1(4) . . ?
N3 C6 C3 123.5(5) . . ?
N2 C6 C3 124.4(5) . . ?
N2 C7 C9 105.7(5) . . ?
N2 C7 C10 110.2(5) . . ?
C9 C7 C10 109.7(6) . . ?
N2 C7 C8 99.3(4) . . ?
C9 C7 C8 115.1(6) . . ?
C10 C7 C8 115.9(5) . . ?
N3 C8 C11 105.5(5) . . ?
N3 C8 C12 109.1(5) . . ?
C11 C8 C12 110.0(6) . . ?
N3 C8 C7 103.6(4) . . ?
C11 C8 C7 113.3(5) . . ?
C12 C8 C7 114.6(6) . . ?
C13 N4 C17 116.2(4) . . ?
C13 N4 Cd1 121.0(3) . . ?
C17 N4 Cd1 122.4(3) . . ?
O3 N5 C18 127.5(5) . . ?
O3 N5 C20 122.6(5) . . ?
C18 N5 C20 109.5(5) . . ?
C18 N6 C19 108.9(5) . . ?
N4 C13 C14 124.4(5) . . ?
C15 C14 C13 118.7(5) . . ?
C14 C15 C16 117.5(5) . . ?
C14 C15 C18 123.4(5) . . ?
C16 C15 C18 119.1(5) . . ?
C17 C16 C15 119.5(5) . . ?
N4 C17 C16 123.6(5) . . ?
N6 C18 N5 112.8(5) . . ?
N6 C18 C15 123.1(5) . . ?
N5 C18 C15 124.1(5) . . ?
C21 C19 N6 110.7(9) . . ?
C21 C19 C20 118.5(10) . . ?
N6 C19 C20 106.0(5) . . ?
C21 C19 C22 119.9(16) . . ?
N6 C19 C22 102.2(7) . . ?
C20 C19 C22 97.3(14) . . ?
C23 C20 N5 116.8(7) . . ?
C23 C20 C19 131.1(8) . . ?
N5 C20 C19 102.3(5) . . ?
C23 C20 C24 97.7(10) . . ?
N5 C20 C24 101.7(8) . . ?
C19 C20 C24 102.0(9) . . ?
C25 N7 Cd1 135.9(4) . . ?
N7 C25 S1 177.6(6) . . ?
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
Cd1 N7 2.312(4) 2 ?
Cd1 N7 2.312(4) . ?
Cd1 N1 2.384(4) . ?
Cd1 N1 2.384(4) 2 ?
Cd1 N4 2.396(4) . ?
Cd1 N4 2.396(4) 2 ?
N1 C5 1.317(7) . ?
N1 C1 1.321(6) . ?
N2 O1 1.277(6) . ?
N2 C6 1.378(7) . ?
N2 C7 1.482(7) . ?
N3 C6 1.303(7) . ?
N3 C8 1.495(7) . ?
C1 C2 1.376(7) . ?
C2 C3 1.369(7) . ?
C3 C4 1.382(7) . ?
C3 C6 1.466(6) . ?
C4 C5 1.367(8) . ?
C7 C9 1.518(9) . ?
C7 C10 1.523(9) . ?
C7 C8 1.549(9) . ?
C8 C11 1.515(9) . ?
C8 C12 1.525(9) . ?
N4 C13 1.317(7) . ?
N4 C17 1.324(7) . ?
N5 O3 1.272(7) . ?
N5 C18 1.374(7) . ?
N5 C20 1.481(7) . ?
N6 C18 1.296(7) . ?
N6 C19 1.490(8) . ?
C13 C14 1.376(7) . ?
C14 C15 1.365(7) . ?
C15 C16 1.376(7) . ?
C15 C18 1.479(7) . ?
C16 C17 1.365(7) . ?
C19 C21 1.400(15) . ?
C19 C20 1.491(11) . ?
C19 C22 1.57(2) . ?
C20 C23 1.389(12) . ?
C20 C24 1.708(16) . ?
S1 C25 1.623(6) . ?
N7 C25 1.107(7) . ?
