#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:46:46 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179262 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/82/4318200.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_4318200
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            'C48 H64 Cd N18 O8'
_chemical_formula_weight         1133.57
_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                90.34(2)
_cell_angle_beta                 102.18(2)
_cell_angle_gamma                91.26(2)
_cell_formula_units_Z            1
_cell_length_a                   7.209(2)
_cell_length_b                   13.802(3)
_cell_length_c                   14.009(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      10.67
_cell_measurement_theta_min      6.11
_cell_volume                     1362.1(6)
_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 0.981
_diffrn_measured_fraction_theta_max 0.981
_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  0.0144
_diffrn_reflns_av_sigmaI/netI    0.0319
_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       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5768
_diffrn_reflns_theta_full        26.14
_diffrn_reflns_theta_max         26.14
_diffrn_reflns_theta_min         1.48
_diffrn_standards_interval_count 250
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.469
_exptl_absorpt_correction_T_max  0.998831
_exptl_absorpt_correction_T_min  0.895229
_exptl_absorpt_correction_type   \y-scan
_exptl_crystal_density_diffrn    1.382
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             590
_refine_diff_density_max         0.832
_refine_diff_density_min         -0.382
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         5321
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0335
_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)+(0.0475P)²+0.4373P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0798
_refine_ls_wR_factor_ref         0.0847
_reflns_number_gt                4701
_reflns_number_total             5321
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020021p_3.cif
_cod_data_source_block           B-293K
_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        1362.1(7)
_cod_database_code               4318200
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
Cd Cd 0.0000 0.0000 0.0000 0.03037(9) Uani 1 2 d S . .
N7 N 0.2413(3) 0.03345(18) -0.07755(17) 0.0467(5) Uani 1 1 d . . .
N8 N 0.2268(3) 0.07939(17) -0.14847(16) 0.0448(5) Uani 1 1 d . . .
N9 N 0.2191(5) 0.1258(3) -0.2173(2) 0.0868(10) Uani 1 1 d . . .
N1 N 0.1295(3) -0.15704(14) 0.03544(15) 0.0371(5) Uani 1 1 d . . .
N2 N 0.5429(3) -0.45167(15) 0.13547(16) 0.0397(5) Uani 1 1 d . . .
N3 N 0.2997(3) -0.47969(14) 0.20371(16) 0.0387(5) Uani 1 1 d . . .
O1 O 0.1493(3) -0.46873(15) 0.23550(17) 0.0575(5) Uani 1 1 d . . .
O2 O 0.6504(3) -0.41515(15) 0.08239(16) 0.0568(5) Uani 1 1 d . . .
C1 C 0.0233(4) -0.23253(18) 0.05478(19) 0.0403(6) Uani 1 1 d . . .
H1 H -0.1074 -0.2253 0.0439 0.048 Uiso 1 1 calc R . .
C2 C 0.0951(4) -0.31965(18) 0.08952(19) 0.0397(6) Uani 1 1 d . . .
H2 H 0.0159 -0.3699 0.1021 0.048 Uiso 1 1 calc R . .
C3 C 0.2894(3) -0.33013(16) 0.10522(17) 0.0341(5) Uani 1 1 d . . .
C4 C 0.4006(4) -0.25267(17) 0.08325(19) 0.0395(6) Uani 1 1 d . . .
H4 H 0.5313 -0.2585 0.0919 0.047 Uiso 1 1 calc R . .
C5 C 0.3167(4) -0.16851(18) 0.04901(19) 0.0400(6) Uani 1 1 d . . .
H5 H 0.3922 -0.1175 0.0347 0.048 Uiso 1 1 calc R . .
C6 C 0.3750(3) -0.41904(17) 0.14608(18) 0.0352(5) Uani 1 1 d . . .
C7 C 0.6039(4) -0.53354(18) 0.20418(19) 0.0407(6) Uani 1 1 d . . .
C8 C 0.4096(4) -0.56998(17) 0.22416(19) 0.0405(6) Uani 1 1 d . . .
C9 C 0.7375(4) -0.4878(2) 0.2930(2) 0.0563(8) Uani 1 1 d . . .
H9A H 0.6698 -0.4419 0.3235 0.084 Uiso 1 1 calc R . .
H9B H 0.8416 -0.4554 0.2726 0.084 Uiso 1 1 calc R . .
H9C H 0.7853 -0.5375 0.3388 0.084 Uiso 1 1 calc R . .
C10 C 0.7068(5) -0.6068(2) 0.1555(2) 0.0580(8) Uani 1 1 d . . .
H10A H 0.6222 -0.6333 0.0987 0.087 Uiso 1 1 calc R . .
H10B H 0.7500 -0.6579 0.2003 0.087 Uiso 1 1 calc R . .
H10C H 0.8138 -0.5757 0.1366 0.087 Uiso 1 1 calc R . .
C11 C 0.4114(5) -0.6018(2) 0.3275(2) 0.0583(8) Uani 1 1 d . . .
H11A H 0.4791 -0.5542 0.3727 0.087 Uiso 1 1 calc R . .
H11B H 0.4729 -0.6629 0.3390 0.087 Uiso 1 1 calc R . .
H11C H 0.2833 -0.6085 0.3365 0.087 Uiso 1 1 calc R . .
C12 C 0.3041(5) -0.6463(2) 0.1504(2) 0.0574(8) Uani 1 1 d . . .
H12A H 0.3037 -0.6252 0.0852 0.086 Uiso 1 1 calc R . .
H12B H 0.1757 -0.6541 0.1586 0.086 Uiso 1 1 calc R . .
H12C H 0.3670 -0.7070 0.1615 0.086 Uiso 1 1 calc R . .
N4 N 0.1998(3) 0.06829(15) 0.14662(14) 0.0370(5) Uani 1 1 d . . .
N5 N 0.7280(3) 0.19974(16) 0.42901(14) 0.0399(5) Uani 1 1 d . . .
N6 N 0.5111(3) 0.14386(16) 0.50505(15) 0.0399(5) Uani 1 1 d . . .
O3 O 0.8119(3) 0.22730(18) 0.36160(14) 0.0622(6) Uani 1 1 d . . .
O4 O 0.3646(3) 0.0989(2) 0.52195(15) 0.0680(7) Uani 1 1 d . . .
C13 C 0.1276(4) 0.09941(19) 0.22068(18) 0.0402(6) Uani 1 1 d . . .
H13 H -0.0038 0.1008 0.2123 0.048 Uiso 1 1 calc R . .
C14 C 0.2362(4) 0.12972(19) 0.30926(18) 0.0398(6) Uani 1 1 d . . .
H14 H 0.1787 0.1511 0.3588 0.048 Uiso 1 1 calc R . .
C15 C 0.4321(3) 0.12795(17) 0.32354(16) 0.0341(5) Uani 1 1 d . . .
C16 C 0.5084(3) 0.09769(19) 0.24618(18) 0.0389(6) Uani 1 1 d . . .
H16 H 0.6393 0.0969 0.2520 0.047 Uiso 1 1 calc R . .
C17 C 0.3885(4) 0.06868(18) 0.16041(17) 0.0386(6) Uani 1 1 d . . .
H17 H 0.4421 0.0482 0.1091 0.046 Uiso 1 1 calc R . .
C18 C 0.5545(3) 0.15708(17) 0.41691(17) 0.0341(5) Uani 1 1 d . . .
C19 C 0.8256(4) 0.2026(2) 0.53539(18) 0.0445(6) Uani 1 1 d . . .
C20 C 0.6535(4) 0.19622(19) 0.58413(17) 0.0401(6) Uani 1 1 d . . .
C21 C 0.9401(4) 0.1111(3) 0.5502(2) 0.0668(9) Uani 1 1 d . . .
H21A H 0.8565 0.0556 0.5341 0.100 Uiso 1 1 calc R . .
H21B H 1.0060 0.1076 0.6172 0.100 Uiso 1 1 calc R . .
H21C H 1.0305 0.1122 0.5087 0.100 Uiso 1 1 calc R . .
C22 C 0.9537(6) 0.2924(3) 0.5581(3) 0.0866(13) Uani 1 1 d . . .
H22A H 0.8777 0.3492 0.5493 0.130 Uiso 1 1 calc R . .
H22B H 1.0407 0.2946 0.5148 0.130 Uiso 1 1 calc R . .
H22C H 1.0235 0.2901 0.6244 0.130 Uiso 1 1 calc R . .
C23 C 0.6806(4) 0.1399(2) 0.6780(2) 0.0566(8) Uani 1 1 d . . .
H23A H 0.7358 0.0787 0.6692 0.085 Uiso 1 1 calc R . .
H23B H 0.5600 0.1292 0.6953 0.085 Uiso 1 1 calc R . .
H23C H 0.7634 0.1762 0.7292 0.085 Uiso 1 1 calc R . .
C24 C 0.5685(5) 0.2935(3) 0.5983(3) 0.0747(11) Uani 1 1 d . . .
H24A H 0.5504 0.3290 0.5385 0.112 Uiso 1 1 calc R . .
H24B H 0.6529 0.3295 0.6490 0.112 Uiso 1 1 calc R . .
H24C H 0.4484 0.2834 0.6165 0.112 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'
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 Cd N7 180.00(9) 2 . ?
N7 Cd N1 91.83(8) 2 . ?
N7 Cd N1 88.17(8) . . ?
N7 Cd N1 88.17(8) 2 2 ?
N7 Cd N1 91.83(8) . 2 ?
N1 Cd N1 180.00(10) . 2 ?
N7 Cd N4 92.44(8) 2 . ?
N7 Cd N4 87.56(8) . . ?
N1 Cd N4 91.60(7) . . ?
N1 Cd N4 88.40(7) 2 . ?
N7 Cd N4 87.56(8) 2 2 ?
N7 Cd N4 92.44(8) . 2 ?
N1 Cd N4 88.40(7) . 2 ?
N1 Cd N4 91.60(7) 2 2 ?
N4 Cd N4 180.00(6) . 2 ?
N8 N7 Cd 124.65(18) . . ?
N9 N8 N7 177.6(3) . . ?
C5 N1 C1 117.7(2) . . ?
C5 N1 Cd 119.83(16) . . ?
C1 N1 Cd 121.89(16) . . ?
O2 N2 C6 126.9(2) . . ?
O2 N2 C7 122.3(2) . . ?
C6 N2 C7 110.5(2) . . ?
O1 N3 C6 127.5(2) . . ?
O1 N3 C8 120.5(2) . . ?
C6 N3 C8 111.9(2) . . ?
N1 C1 C2 124.2(2) . . ?
C1 C2 C3 117.6(2) . . ?
C2 C3 C4 118.5(2) . . ?
C2 C3 C6 120.3(2) . . ?
C4 C3 C6 121.1(2) . . ?
C5 C4 C3 119.7(2) . . ?
N1 C5 C4 122.1(2) . . ?
N2 C6 N3 109.6(2) . . ?
N2 C6 C3 125.5(2) . . ?
N3 C6 C3 124.9(2) . . ?
N2 C7 C10 109.5(2) . . ?
N2 C7 C9 105.7(2) . . ?
C10 C7 C9 110.5(2) . . ?
N2 C7 C8 101.23(19) . . ?
C10 C7 C8 114.9(2) . . ?
C9 C7 C8 114.2(2) . . ?
N3 C8 C11 109.4(2) . . ?
N3 C8 C12 105.8(2) . . ?
C11 C8 C12 110.3(2) . . ?
N3 C8 C7 99.71(19) . . ?
C11 C8 C7 115.8(2) . . ?
C12 C8 C7 114.7(2) . . ?
C13 N4 C17 116.7(2) . . ?
C13 N4 Cd 121.60(16) . . ?
C17 N4 Cd 121.47(16) . . ?
O3 N5 C18 126.8(2) . . ?
O3 N5 C19 122.1(2) . . ?
C18 N5 C19 110.8(2) . . ?
O4 N6 C18 126.4(2) . . ?
O4 N6 C20 122.6(2) . . ?
C18 N6 C20 110.9(2) . . ?
N4 C13 C14 123.8(2) . . ?
C13 C14 C15 119.1(2) . . ?
C16 C15 C14 117.5(2) . . ?
C16 C15 C18 121.0(2) . . ?
C14 C15 C18 121.5(2) . . ?
C17 C16 C15 119.2(2) . . ?
N4 C17 C16 123.7(2) . . ?
N5 C18 N6 109.2(2) . . ?
N5 C18 C15 125.9(2) . . ?
N6 C18 C15 124.8(2) . . ?
N5 C19 C21 104.7(2) . . ?
N5 C19 C22 110.5(2) . . ?
C21 C19 C22 111.1(3) . . ?
N5 C19 C20 100.76(19) . . ?
C21 C19 C20 111.8(2) . . ?
C22 C19 C20 116.9(3) . . ?
N6 C20 C23 110.0(2) . . ?
N6 C20 C24 106.0(2) . . ?
C23 C20 C24 109.5(2) . . ?
N6 C20 C19 100.39(18) . . ?
C23 C20 C19 116.1(2) . . ?
C24 C20 C19 114.0(3) . . ?
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
Cd N7 2.278(2) 2 ?
Cd N7 2.278(2) . ?
Cd N1 2.392(2) . ?
Cd N1 2.392(2) 2 ?
Cd N4 2.419(2) . ?
Cd N4 2.419(2) 2 ?
N7 N8 1.169(3) . ?
N8 N9 1.153(3) . ?
N1 C5 1.335(3) . ?
N1 C1 1.342(3) . ?
N2 O2 1.279(3) . ?
N2 C6 1.338(3) . ?
N2 C7 1.501(3) . ?
N3 O1 1.268(3) . ?
N3 C6 1.349(3) . ?
N3 C8 1.488(3) . ?
C1 C2 1.371(3) . ?
C2 C3 1.382(3) . ?
C3 C4 1.397(3) . ?
C3 C6 1.452(3) . ?
C4 C5 1.364(3) . ?
C7 C10 1.508(4) . ?
C7 C9 1.527(4) . ?
C7 C8 1.559(4) . ?
C8 C11 1.513(4) . ?
C8 C12 1.541(4) . ?
N4 C13 1.328(3) . ?
N4 C17 1.333(3) . ?
N5 O3 1.280(3) . ?
N5 C18 1.348(3) . ?
N5 C19 1.508(3) . ?
N6 O4 1.279(3) . ?
N6 C18 1.349(3) . ?
N6 C20 1.510(3) . ?
C13 C14 1.377(3) . ?
C14 C15 1.384(3) . ?
C15 C16 1.381(3) . ?
C15 C18 1.464(3) . ?
C16 C17 1.376(3) . ?
C19 C21 1.515(4) . ?
C19 C22 1.520(4) . ?
C19 C20 1.538(4) . ?
C20 C23 1.511(4) . ?
C20 C24 1.517(4) . ?
