#------------------------------------------------------------------------------
#$Date: 2016-03-26 21:00:41 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180460 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/29/7212964.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# 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_7212964
loop_
_publ_author_name
'Azcondo, M. Teresa'
'Ballester, Loreto'
'Golhen, Stephane'
'Gutierrez, Angel'
'Ouahab, Lahcene'
'Yartsev, Slav'
'Delhaes, Pierre'
_publ_section_title
;
 Structural, magnetic, electrical and optical characterization of systems
 built from [M([9]aneN3)2]2+ (M=CuII or NiII) and TCNQ or TCNQF4
;
_journal_issue                   6
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              1237
_journal_paper_doi               10.1039/a807595f
_journal_volume                  9
_journal_year                    1999
_chemical_formula_moiety         '[Cu[9]aneN3)2](TCNQ)3'
_chemical_formula_sum            'C48 H42 Cu N18'
_chemical_formula_weight         934.54
_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
_cell_angle_alpha                74.10(2)
_cell_angle_beta                 89.01(2)
_cell_angle_gamma                69.11(2)
_cell_formula_units_Z            1
_cell_length_a                   8.350(2)
_cell_length_b                   9.884(4)
_cell_length_c                   14.369(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_volume                     1061.3(6)
_computing_cell_refinement       'Enraf Nonius'
_computing_data_collection       'Enraf Nonius CAD4'
_computing_data_reduction        MolEN
_computing_molecular_graphics    ORTEP
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       '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  0.0090
_diffrn_reflns_av_sigmaI/netI    0.0213
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            4871
_diffrn_reflns_theta_max         26.97
_diffrn_reflns_theta_min         1.48
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 250
_diffrn_standards_interval_time  3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.576
_exptl_absorpt_correction_T_max  0.99878
_exptl_absorpt_correction_T_min  0.908442
_exptl_absorpt_correction_type   \y-scan
_exptl_crystal_colour            'deep blue'
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_F_000             485
_refine_diff_density_max         0.270
_refine_diff_density_min         -0.476
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.055
_refine_ls_goodness_of_fit_obs   1.058
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         4546
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_restrained_S_obs      1.058
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_obs          0.0311
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0571P)²+0.1996P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0891
_refine_ls_wR_factor_obs         0.0829
_reflns_number_observed          3961
_reflns_number_total             4546
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            807595fsup1.cif
_cod_data_source_block           cutq3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0571P)^2^+0.1996P] 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^)+(0.0571P)^2^+0.1996P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1061.2(6)
_cod_database_code               7212964
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
Cu Cu 0.0000 0.0000 0.0000 0.02275(9) Uani 1 d S
N1 N 0.2012(2) 0.0577(2) 0.03171(10) 0.0317(3) Uani 1 d .
N2 N 0.0094(2) 0.1237(2) -0.13911(10) 0.0279(3) Uani 1 d .
N3 N -0.1522(2) 0.2510(2) 0.00754(12) 0.0364(3) Uani 1 d .
C1 C 0.2964(2) 0.0561(2) -0.05612(14) 0.0369(4) Uani 1 d .
C2 C 0.1752(2) 0.1479(2) -0.14713(13) 0.0343(4) Uani 1 d .
C3 C -0.1414(2) 0.2675(2) -0.16634(13) 0.0351(4) Uani 1 d .
C4 C -0.1630(3) 0.3518(2) -0.09066(14) 0.0375(4) Uani 1 d .
C5 C -0.0366(3) 0.2621(2) 0.07808(14) 0.0434(5) Uani 1 d .
C6 C 0.1508(3) 0.2035(2) 0.05575(15) 0.0419(5) Uani 1 d .
N4 N 0.4222(2) 0.8798(2) 0.23658(11) 0.0421(4) Uani 1 d .
N5 N 0.9137(2) 0.6648(2) 0.40526(13) 0.0474(4) Uani 1 d .
N6 N -0.0714(2) 0.6069(2) 0.72611(13) 0.0477(4) Uani 1 d .
N7 N 0.4223(3) 0.3827(2) 0.89602(13) 0.0544(5) Uani 1 d .
C7 C 0.5049(2) 0.6855(2) 0.48541(11) 0.0238(3) Uani 1 d .
C8 C 0.3225(2) 0.7225(2) 0.47893(12) 0.0268(3) Uani 1 d .
C9 C 0.2421(2) 0.6804(2) 0.55794(12) 0.0278(3) Uani 1 d .
C10 C 0.3359(2) 0.5983(2) 0.65088(11) 0.0253(3) Uani 1 d .
C11 C 0.5169(2) 0.5633(2) 0.65715(11) 0.0266(3) Uani 1 d .
C12 C 0.5992(2) 0.6033(2) 0.57820(11) 0.0255(3) Uani 1 d .
C13 C 0.5876(2) 0.7289(2) 0.40373(11) 0.0263(3) Uani 1 d .
C14 C 0.4941(2) 0.8130(2) 0.31114(12) 0.0295(3) Uani 1 d .
C15 C 0.7686(2) 0.6921(2) 0.40606(12) 0.0307(4) Uani 1 d .
C16 C 0.2540(2) 0.5491(2) 0.73188(12) 0.0291(3) Uani 1 d .
C17 C 0.0733(2) 0.5829(2) 0.72735(12) 0.0323(4) Uani 1 d .
C18 C 0.3475(2) 0.4588(2) 0.82308(13) 0.0343(4) Uani 1 d .
N8 N 0.9947(2) 0.0175(2) 0.33233(14) 0.0516(5) Uani 1 d .
N9 N 0.5195(3) 0.2427(2) 0.16502(12) 0.0539(5) Uani 1 d .
C19 C 0.5846(2) 0.0445(2) 0.41721(11) 0.0239(3) Uani 1 d .
C20 C 0.4033(2) 0.0831(2) 0.41113(11) 0.0248(3) Uani 1 d .
C21 C 0.6782(2) -0.0398(2) 0.50972(11) 0.0249(3) Uani 1 d .
C22 C 0.6688(2) 0.0901(2) 0.33574(11) 0.0269(3) Uani 1 d .
C23 C 0.8495(2) 0.0481(2) 0.33722(12) 0.0324(4) Uani 1 d .
C24 C 0.5807(2) 0.1750(2) 0.24206(12) 0.0327(4) Uani 1 d .
H1 H 0.2671(29) -0.0102(26) 0.0782(16) 0.041(6) Uiso 1 d .
H2 H 0.3871(27) 0.0949(23) -0.0576(14) 0.037(5) Uiso 1 d .
H3 H 0.3533(27) -0.0523(25) -0.0549(15) 0.037(5) Uiso 1 d .
H4 H 0.1502(26) 0.2533(25) -0.1553(15) 0.038(5) Uiso 1 d .
H5 H 0.2373(30) 0.1088(26) -0.2007(17) 0.050(6) Uiso 1 d .
H6 H 0.0050(28) 0.0751(25) -0.1813(16) 0.041(6) Uiso 1 d .
H7 H -0.1302(25) 0.3310(23) -0.2297(15) 0.033(5) Uiso 1 d .
H8 H -0.2398(29) 0.2404(24) -0.1722(15) 0.042(6) Uiso 1 d .
H9 H -0.0827(26) 0.3963(22) -0.0949(14) 0.030(5) Uiso 1 d .
H10 H -0.2717(29) 0.4357(26) -0.1055(16) 0.044(6) Uiso 1 d .
H11 H -0.2560(33) 0.2690(28) 0.0281(18) 0.055(7) Uiso 1 d .
H12 H -0.0439(32) 0.2023(29) 0.1451(19) 0.061(7) Uiso 1 d .
H13 H -0.0656(27) 0.3601(26) 0.0827(15) 0.039(5) Uiso 1 d .
H14 H 0.1704(28) 0.2729(26) 0.0047(17) 0.043(6) Uiso 1 d .
H15 H 0.2260(31) 0.1930(27) 0.1096(18) 0.052(6) Uiso 1 d .
H16 H 0.2623(25) 0.7783(22) 0.4176(14) 0.030(5) Uiso 1 d .
H17 H 0.1211(30) 0.7038(25) 0.5549(15) 0.043(6) Uiso 1 d .
H18 H 0.5764(26) 0.5138(23) 0.7203(15) 0.034(5) Uiso 1 d .
H19 H 0.7195(25) 0.5769(21) 0.5825(13) 0.027(5) Uiso 1 d .
H20 H 0.3416(25) 0.1403(22) 0.3501(15) 0.032(5) Uiso 1 d .
H21 H 0.7993(26) -0.0649(21) 0.5137(14) 0.030(5) Uiso 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'
Cu Cu 0.3201 1.2651 '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
N1 Cu N1 180.0 2 .
N1 Cu N2 96.12(6) 2 .
N1 Cu N2 83.88(6) . .
N1 Cu N2 83.88(6) 2 2
N1 Cu N2 96.12(6) . 2
N2 Cu N2 180.0 . 2
N1 Cu N3 100.33(6) 2 .
N1 Cu N3 79.67(6) . .
N2 Cu N3 78.76(6) . .
N2 Cu N3 101.24(6) 2 .
N1 Cu N3 79.67(6) 2 2
N1 Cu N3 100.33(6) . 2
N2 Cu N3 101.24(6) . 2
N2 Cu N3 78.76(6) 2 2
N3 Cu N3 180.0 . 2
C1 N1 C6 113.21(15) . .
C1 N1 Cu 102.84(11) . .
C6 N1 Cu 115.04(12) . .
C3 N2 C2 112.45(14) . .
C3 N2 Cu 110.10(11) . .
C2 N2 Cu 109.63(10) . .
C5 N3 C4 113.5(2) . .
C5 N3 Cu 100.46(12) . .
C4 N3 Cu 106.65(11) . .
N1 C1 C2 110.60(14) . .
N2 C2 C1 111.26(14) . .
N2 C3 C4 111.78(14) . .
N3 C4 C3 111.12(15) . .
N3 C5 C6 112.0(2) . .
N1 C6 C5 112.9(2) . .
C13 C7 C8 120.94(14) . .
C13 C7 C12 121.13(15) . .
C8 C7 C12 117.93(14) . .
C9 C8 C7 121.05(15) . .
C8 C9 C10 121.2(2) . .
C16 C10 C11 121.17(15) . .
C16 C10 C9 121.3(2) . .
C11 C10 C9 117.50(14) . .
C12 C11 C10 121.80(15) . .
C11 C12 C7 120.5(2) . .
C7 C13 C15 123.01(15) . .
C7 C13 C14 121.5(2) . .
C15 C13 C14 115.45(15) . .
N4 C14 C13 178.8(2) . .
N5 C15 C13 178.1(2) . .
C10 C16 C18 121.8(2) . .
C10 C16 C17 122.1(2) . .
C18 C16 C17 116.04(15) . .
N6 C17 C16 178.1(2) . .
N7 C18 C16 178.1(2) . .
C22 C19 C20 121.42(15) . .
C22 C19 C21 121.0(2) . .
C20 C19 C21 117.57(14) . .
C21 C20 C19 121.36(15) 2_656 .
C20 C21 C19 121.1(2) 2_656 .
C19 C22 C23 123.3(2) . .
C19 C22 C24 123.0(2) . .
C23 C22 C24 113.50(15) . .
N8 C23 C22 175.8(2) . .
N9 C24 C22 175.9(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu N1 2.0512(15) 2
Cu N1 2.0512(15) .
Cu N2 2.054(2) .
Cu N2 2.054(2) 2
Cu N3 2.382(2) .
Cu N3 2.382(2) 2
N1 C1 1.481(2) .
N1 C6 1.486(3) .
N2 C3 1.481(2) .
N2 C2 1.484(2) .
N3 C5 1.463(3) .
N3 C4 1.470(2) .
C1 C2 1.516(3) .
C3 C4 1.513(3) .
C5 C6 1.525(3) .
N4 C14 1.139(2) .
N5 C15 1.144(2) .
N6 C17 1.144(3) .
N7 C18 1.145(3) .
C7 C13 1.395(2) .
C7 C8 1.432(2) .
C7 C12 1.430(2) .
C8 C9 1.351(2) .
C9 C10 1.430(2) .
C10 C16 1.399(2) .
C10 C11 1.424(2) .
C11 C12 1.355(2) .
C13 C15 1.421(2) .
C13 C14 1.427(2) .
C16 C18 1.422(2) .
C16 C17 1.423(2) .
N8 C23 1.146(3) .
N9 C24 1.142(2) .
C19 C22 1.406(2) .
C19 C20 1.421(2) .
C19 C21 1.427(2) .
C20 C21 1.362(2) 2_656
C21 C20 1.362(2) 2_656
C22 C23 1.414(2) .
C22 C24 1.425(2) .
