#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/15/2211534.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2211534
loop_
_publ_author_name
'Aliakbar Dehno Khalaji'
'Mehdi Amirnasr'
'Jean-Claude Daran'
_publ_section_title
;Bis[N,N'-bis(3,3-diphenylprop-2-enylidene)ethane-1,2-diamine-κ²N,N']copper(I)
 triiodide
;
_journal_coeditor_code           NG2135
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m3183
_journal_page_last               m3184
_journal_paper_doi               10.1107/S1600536806044916
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Cu (C32 H28 N2)2] I3'
_chemical_formula_moiety         'C64 H56 Cu N4 + , I3 -'
_chemical_formula_sum            'C64 H56 Cu I3 N4'
_chemical_formula_weight         1325.38
_chemical_name_systematic
;Bis[N,N'-bis(3,3-diphenylprop-2-enylidene)ethane-1,2-diamine-κ²N,N']copper(I)
triiodide
;
_space_group_IT_number           118
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P -4 -2n'
_symmetry_space_group_name_H-M   'P -4 n 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.1304(7)
_cell_length_b                   17.1304(7)
_cell_length_c                   9.6273(4)
_cell_measurement_reflns_used    11035
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      32.02
_cell_measurement_theta_min      2.7
_cell_volume                     2825.1(2)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlis RED'
_computing_molecular_graphics
;
ORTEPIII (Burnett & Johnson, 1996) and ORTEP-3 for Windows (Farrugia,
1997)
;
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al.,  1999)'
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean 8.2632
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Oxford XCALIBUR'
_diffrn_measurement_method       'φ and ω'
_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  0.0236
_diffrn_reflns_av_sigmaI/netI    0.0188
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            29420
_diffrn_reflns_theta_full        32.01
_diffrn_reflns_theta_max         32.01
_diffrn_reflns_theta_min         2.66
_exptl_absorpt_coefficient_mu    2.069
_exptl_absorpt_correction_T_max  0.821
_exptl_absorpt_correction_T_min  0.678
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlis RED; Oxford Diffraction, 2006)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.558
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.32
_refine_diff_density_max         1.038
_refine_diff_density_min         -0.726
_refine_ls_abs_structure_details
;
Flack (1983) and Bernardinelli & Flack (1985), using 2109
Friedel pairs
;
_refine_ls_abs_structure_Flack   -0.031(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     165
_refine_ls_number_reflns         4735
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0320
_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)+(0.0211P)²+1.9967P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0615
_refine_ls_wR_factor_ref         0.0686
_reflns_number_gt                3587
_reflns_number_total             4735
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ng2135.cif
_cod_data_source_block           I
_cod_database_code               2211534
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-y+1/2, -x+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-y, x, -z'
'y, -x, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
C C1 -0.10339(13) 0.37530(14) 0.1759(3) 0.0367(6) Uani d . 1
H H1A -0.1095 0.3184 0.1616 0.044 Uiso calc R 1
H H1B -0.1383 0.4028 0.1100 0.044 Uiso calc R 1
C C11 0.02211(14) 0.34988(14) 0.0877(3) 0.0271(5) Uani d . 1
H H11 0.0026 0.2999 0.0628 0.033 Uiso calc R 1
C C12 0.10134(13) 0.37033(13) 0.0531(2) 0.0274(5) Uani d . 1
H H12 0.1151 0.4240 0.0555 0.033 Uiso calc R 1
C C13 0.15754(12) 0.31876(12) 0.0176(2) 0.0236(5) Uani d . 1
C C131 0.14578(14) 0.23369(14) 0.0368(3) 0.0252(5) Uani d . 1
C C132 0.11750(15) 0.20465(15) 0.1617(3) 0.0319(5) Uani d . 1
H H132 0.1057 0.2397 0.2354 0.038 Uiso calc R 1
C C133 0.10618(18) 0.12488(16) 0.1803(3) 0.0397(7) Uani d . 1
H H133 0.0868 0.1055 0.2662 0.048 Uiso calc R 1
C C134 0.12333(19) 0.07372(16) 0.0727(3) 0.0432(7) Uani d . 1
H H134 0.1154 0.0192 0.0843 0.052 Uiso calc R 1
C C135 0.15180(19) 0.10206(17) -0.0506(3) 0.0367(7) Uani d . 1
H H135 0.1635 0.0668 -0.1238 0.044 Uiso calc R 1
C C136 0.16364(14) 0.18091(15) -0.0697(3) 0.0289(5) Uani d . 1
H H136 0.1840 0.1995 -0.1554 0.035 Uiso calc R 1
C C141 0.23381(15) 0.34646(15) -0.0324(3) 0.0294(5) Uani d . 1
C C142 0.30174(16) 0.3029(2) -0.0094(3) 0.0423(6) Uani d . 1
H H142 0.2987 0.2528 0.0327 0.051 Uiso calc R 1
C C143 0.3736(2) 0.3332(3) -0.0484(5) 0.0687(15) Uani d . 1
H H143 0.4195 0.3035 -0.0323 0.082 Uiso calc R 1
C C144 0.3795(3) 0.4043(3) -0.1091(5) 0.0850(18) Uani d . 1
H H144 0.4293 0.4249 -0.1326 0.102 Uiso calc R 1
C C145 0.3133(3) 0.4465(2) -0.1362(4) 0.0736(14) Uani d . 1
H H145 0.3174 0.4959 -0.1804 0.088 Uiso calc R 1
C C146 0.2405(2) 0.41798(18) -0.0998(3) 0.0466(8) Uani d . 1
H H146 0.1950 0.4473 -0.1209 0.056 Uiso calc R 1
N N1 -0.02260(11) 0.39815(11) 0.1515(2) 0.0246(4) Uani d . 1
Cu Cu1 0.0000 0.5000 0.2500 0.02255(9) Uani d S 1
I I1 0.0000 0.5000 0.7500 0.04172(8) Uani d S 1
I I2 -0.120456(12) 0.379544(12) 0.7500 0.06406(10) Uani d S 1
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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
N1 C1 C1 . 4_455 108.37(18)
N1 C1 H1A . . 110.0
N1 C1 H1B . . 110.0
H1A C1 H1B . . 108.4
N1 C11 C12 . . 121.1(2)
N1 C11 H11 . . 119.5
C12 C11 H11 . . 119.5
C13 C12 C11 . . 124.8(2)
C13 C12 H12 . . 117.6
C11 C12 H12 . . 117.6
C12 C13 C141 . . 120.3(2)
C12 C13 C131 . . 121.0(2)
C141 C13 C131 . . 118.6(2)
C132 C131 C136 . . 118.6(2)
C132 C131 C13 . . 120.5(2)
C136 C131 C13 . . 120.9(2)
C131 C132 C133 . . 120.8(3)
C131 C132 H132 . . 119.6
C133 C132 H132 . . 119.6
C134 C133 C132 . . 119.6(3)
C134 C133 H133 . . 120.2
C132 C133 H133 . . 120.2
C135 C134 C133 . . 119.8(3)
C135 C134 H134 . . 120.1
C133 C134 H134 . . 120.1
C134 C135 C136 . . 121.0(3)
C134 C135 H135 . . 119.5
C136 C135 H135 . . 119.5
C135 C136 C131 . . 120.2(3)
C135 C136 H136 . . 119.9
C131 C136 H136 . . 119.9
C146 C141 C142 . . 118.3(3)
C146 C141 C13 . . 120.7(3)
C142 C141 C13 . . 121.0(2)
C143 C142 C141 . . 119.7(4)
C143 C142 H142 . . 120.2
C141 C142 H142 . . 120.2
C144 C143 C142 . . 121.3(4)
C144 C143 H143 . . 119.4
C142 C143 H143 . . 119.4
C143 C144 C145 . . 119.6(3)
C143 C144 H144 . . 120.2
C145 C144 H144 . . 120.2
C144 C145 C146 . . 120.8(4)
C144 C145 H145 . . 119.6
C146 C145 H145 . . 119.6
C145 C146 C141 . . 120.2(4)
C145 C146 H146 . . 119.9
C141 C146 H146 . . 119.9
C11 N1 C1 . . 118.1(2)
C11 N1 Cu1 . . 131.74(17)
C1 N1 Cu1 . . 109.75(14)
N1 Cu1 N1 . 3 123.35(11)
N1 Cu1 N1 . 4_455 83.67(11)
N1 Cu1 N1 3 4_455 124.09(12)
N1 Cu1 N1 . 2_565 124.09(12)
N1 Cu1 N1 3 2_565 83.67(11)
N1 Cu1 N1 4_455 2_565 123.35(11)
I2 I1 I2 2_565 . 180.0
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
C1 N1 . 1.457(3)
C1 C1 4_455 1.518(6)
C1 H1A . 0.9900
C1 H1B . 0.9900
C11 N1 . 1.284(3)
C11 C12 . 1.441(3)
C11 H11 . 0.9500
C12 C13 . 1.351(3)
C12 H12 . 0.9500
C13 C141 . 1.471(3)
C13 C131 . 1.483(3)
C131 C132 . 1.389(4)
C131 C136 . 1.401(3)
C132 C133 . 1.392(4)
C132 H132 . 0.9500
C133 C134 . 1.389(4)
C133 H133 . 0.9500
C134 C135 . 1.371(5)
C134 H134 . 0.9500
C135 C136 . 1.378(4)
C135 H135 . 0.9500
C136 H136 . 0.9500
C141 C146 . 1.391(4)
C141 C142 . 1.400(4)
C142 C143 . 1.388(5)
C142 H142 . 0.9500
C143 C144 . 1.355(8)
C143 H143 . 0.9500
C144 C145 . 1.369(7)
C144 H144 . 0.9500
C145 C146 . 1.385(5)
C145 H145 . 0.9500
C146 H146 . 0.9500
N1 Cu1 . 2.0232(19)
Cu1 N1 3 2.0232(19)
I1 I2 . 2.9182(3)
