#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/35/7003587.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_7003587
loop_
_publ_author_name
'Yuste, C.'
'Armentano, D.'
'Marino, N.'
'Cañadillas-Delgado, L.'
'Delgado, F. S.'
'Ruiz-Pérez, C.'
'Rillema, D. P.'
'Lloret, F.'
'Julve, M.'
_publ_section_title
;
 Synthesis, crystal structures and magnetic properties of
 tricyanomethanide-containing copper(II) complexes
;
_journal_issue                   12
_journal_name_full               'Dalton Transactions'
_journal_page_first              1583
_journal_page_last               1596
_journal_paper_doi               10.1039/b717347d
_journal_year                    2008
_chemical_formula_sum            'C40 H19 Cu2 N18 O1.5'
_chemical_formula_weight         902.81
_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                80.965(6)
_cell_angle_beta                 88.684(6)
_cell_angle_gamma                89.289(4)
_cell_formula_units_Z            2
_cell_length_a                   9.8741(6)
_cell_length_b                   12.8989(7)
_cell_length_c                   16.0258(8)
_cell_measurement_temperature    293(2)
_cell_volume                     2015.2(2)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           Mok\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_sigmaI/netI    0.0897
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18852
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         6.41
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    1.115
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            braun
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       sheet
_exptl_crystal_F_000             910
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.336
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     623
_refine_ls_number_reflns         8862
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.1248
_refine_ls_R_factor_gt           0.0570
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0271P)²+1.8728P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0890
_refine_ls_wR_factor_ref         0.1073
_reflns_number_gt                5267
_reflns_number_total             8862
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b717347d.txt
_cod_data_source_block           ull1339=ull1337
_cod_original_cell_volume        2015.19(19)
_cod_original_formula_sum        'C40 H19 Cu2 N18 O1.50'
_cod_database_code               7003587
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
Cu1 Cu 0.83396(5) 0.48173(3) 0.73105(3) 0.03422(14) Uani 1 1 d . . .
Cu2 Cu 0.53598(5) 0.93051(3) 0.76216(3) 0.03677(14) Uani 1 1 d . . .
N1 N 0.8138(3) 0.5400(2) 0.60874(17) 0.0320(7) Uani 1 1 d . . .
N2 N 0.8123(3) 0.4664(2) 0.85713(17) 0.0325(7) Uani 1 1 d . . .
N4 N 0.5145(3) 0.8593(2) 0.88210(18) 0.0372(7) Uani 1 1 d . . .
N3 N 0.6012(3) 0.9602(2) 0.64215(19) 0.0432(8) Uani 1 1 d . . .
N5 N 0.7480(3) 0.61716(19) 0.74155(16) 0.0243(6) Uani 1 1 d . . .
N6 N 0.6327(3) 0.79844(19) 0.75490(16) 0.0253(6) Uani 1 1 d . . .
C1 C 0.8365(5) 0.4860(3) 0.5453(3) 0.0471(10) Uani 1 1 d . . .
C2 C 0.7978(6) 0.5231(4) 0.4645(3) 0.0627(14) Uani 1 1 d . . .
C3 C 0.7299(6) 0.6161(4) 0.4485(3) 0.0641(14) Uani 1 1 d . . .
C4 C 0.7049(4) 0.6733(3) 0.5139(2) 0.0448(10) Uani 1 1 d . . .
C5 C 0.7502(3) 0.6348(2) 0.5929(2) 0.0280(8) Uani 1 1 d . . .
C6 C 0.7707(3) 0.5545(3) 0.8860(2) 0.0284(8) Uani 1 1 d . . .
C7 C 0.7877(4) 0.5669(3) 0.9691(2) 0.0386(9) Uani 1 1 d . . .
C8 C 0.8391(4) 0.4829(4) 1.0247(3) 0.0489(11) Uani 1 1 d . . .
C9 C 0.8740(4) 0.3925(4) 0.9971(3) 0.0541(13) Uani 1 1 d . . .
C10 C 0.8642(4) 0.3868(3) 0.9121(3) 0.0462(11) Uani 1 1 d . . .
C11 C 0.6818(4) 0.8845(2) 0.6175(2) 0.0348(9) Uani 1 1 d . . .
C12 C 0.7632(5) 0.9044(3) 0.5458(3) 0.0489(11) Uani 1 1 d . . .
C13 C 0.7561(7) 1.0029(4) 0.4964(3) 0.0768(17) Uani 1 1 d . . .
C14 C 0.6680(7) 1.0768(4) 0.5186(3) 0.0804(19) Uani 1 1 d . . .
C15 C 0.5933(6) 1.0535(3) 0.5919(3) 0.0655(15) Uani 1 1 d . . .
C16 C 0.4386(5) 0.8958(3) 0.9408(3) 0.0517(11) Uani 1 1 d . . .
C17 C 0.4007(5) 0.8344(4) 1.0154(3) 0.0529(12) Uani 1 1 d . . .
C18 C 0.4395(4) 0.7315(3) 1.0290(2) 0.0405(10) Uani 1 1 d . . .
C19 C 0.5173(4) 0.6921(3) 0.9688(2) 0.0335(8) Uani 1 1 d . . .
C20 C 0.5574(4) 0.7576(3) 0.8962(2) 0.0292(8) Uani 1 1 d . . .
C21 C 0.7270(3) 0.6840(2) 0.6695(2) 0.0263(8) Uani 1 1 d . . .
C22 C 0.6829(4) 0.7857(2) 0.6790(2) 0.0283(8) Uani 1 1 d . . .
C23 C 0.6379(3) 0.7268(2) 0.82504(19) 0.0241(7) Uani 1 1 d . . .
C24 C 0.7153(3) 0.6360(2) 0.8192(2) 0.0240(7) Uani 1 1 d . . .
N32 N 0.8909(4) 0.3393(2) 0.7210(2) 0.0529(9) Uani 1 1 d . . .
N33 N 1.2110(6) 0.1327(4) 0.6554(3) 0.0922(16) Uani 1 1 d . . .
N34 N 0.8102(6) 0.0052(4) 0.7700(5) 0.146(3) Uani 1 1 d . . .
C31 C 0.9722(6) 0.1536(3) 0.7154(3) 0.0628(13) Uani 1 1 d . . .
C32 C 0.9272(4) 0.2558(3) 0.7186(3) 0.0492(11) Uani 1 1 d . . .
C33 C 1.1034(7) 0.1399(4) 0.6819(4) 0.0697(16) Uani 1 1 d . . .
C34 C 0.8841(6) 0.0705(4) 0.7450(4) 0.091(2) Uani 1 1 d . . .
N36 N 1.0539(4) 0.5360(2) 0.74155(19) 0.0439(8) Uani 1 1 d . . .
N37 N 1.4187(4) 0.6879(3) 0.6154(2) 0.0632(11) Uani 1 1 d . . .
N38 N 1.4506(4) 0.5052(3) 0.8697(2) 0.0493(9) Uani 1 1 d . . .
C35 C 1.3059(4) 0.5746(3) 0.7422(2) 0.0343(8) Uani 1 1 d . . .
C36 C 1.1671(4) 0.5534(3) 0.7425(2) 0.0324(8) Uani 1 1 d . . .
C37 C 1.3674(4) 0.6369(3) 0.6717(3) 0.0432(10) Uani 1 1 d . . .
C38 C 1.3842(4) 0.5363(3) 0.8131(2) 0.0361(9) Uani 1 1 d . . .
N40 N 0.4953(4) 1.0737(2) 0.7800(2) 0.0501(9) Uani 1 1 d . . .
N42 N 0.5887(4) 1.4038(3) 0.7089(3) 0.0698(12) Uani 1 1 d . . .
N41 N 0.2029(5) 1.3023(3) 0.8508(3) 0.0784(13) Uani 1 1 d . . .
C39 C 0.4242(4) 1.2632(3) 0.7765(2) 0.0365(9) Uani 1 1 d . . .
C40 C 0.4614(4) 1.1593(3) 0.7775(2) 0.0389(9) Uani 1 1 d . . .
C41 C 0.3012(5) 1.2862(3) 0.8161(3) 0.0455(10) Uani 1 1 d . . .
C42 C 0.5144(4) 1.3414(3) 0.7392(2) 0.0429(10) Uani 1 1 d . . .
N44 N 0.3322(4) 0.8851(3) 0.7352(2) 0.0590(10) Uani 1 1 d . . .
N46 N 0.0438(5) 0.7506(4) 0.5757(3) 0.0882(16) Uani 1 1 d . . .
N45 N -0.0561(5) 0.7727(3) 0.8446(3) 0.0791(14) Uani 1 1 d . . .
C43 C 0.1011(4) 0.8104(3) 0.7145(3) 0.0555(12) Uani 1 1 d . . .
C44 C 0.2277(5) 0.8523(3) 0.7258(3) 0.0489(11) Uani 1 1 d . . .
C45 C 0.0137(5) 0.7900(3) 0.7852(4) 0.0614(14) Uani 1 1 d . . .
C46 C 0.0695(5) 0.7776(4) 0.6372(4) 0.0637(14) Uani 1 1 d . . .
O1W O 0.9781(16) 0.1424(9) 0.9448(10) 0.202(6) Uani 0.50 1 d P . .
O2W O 0.2056(11) 1.0695(10) 1.0266(8) 0.316(6) Uani 1 1 d . . .
H1 H 0.884(4) 0.420(3) 0.557(2) 0.037(10) Uiso 1 1 d . . .
H2 H 0.821(5) 0.481(4) 0.426(3) 0.075(15) Uiso 1 1 d . . .
H3 H 0.698(5) 0.645(4) 0.396(3) 0.094(18) Uiso 1 1 d . . .
H4 H 0.651(4) 0.733(3) 0.506(2) 0.052(12) Uiso 1 1 d . . .
H7 H 0.762(3) 0.628(2) 0.9848(19) 0.020(9) Uiso 1 1 d . . .
H8 H 0.856(4) 0.499(3) 1.077(2) 0.041(11) Uiso 1 1 d . . .
H9 H 0.912(4) 0.337(3) 1.031(3) 0.070(14) Uiso 1 1 d . . .
H10 H 0.891(4) 0.324(3) 0.887(2) 0.040(10) Uiso 1 1 d . . .
H12 H 0.824(4) 0.857(3) 0.535(2) 0.039(11) Uiso 1 1 d . . .
H13 H 0.810(4) 1.016(3) 0.451(3) 0.059(13) Uiso 1 1 d . . .
H14 H 0.659(5) 1.136(4) 0.488(3) 0.073(14) Uiso 1 1 d . . .
H15 H 0.537(4) 1.099(3) 0.615(2) 0.054(13) Uiso 1 1 d . . .
H16 H 0.408(4) 0.961(3) 0.926(2) 0.045(11) Uiso 1 1 d . . .
H17 H 0.349(4) 0.861(3) 1.050(2) 0.049(12) Uiso 1 1 d . . .
H19 H 0.412(3) 0.687(3) 1.072(2) 0.031(10) Uiso 1 1 d . . .
H18 H 0.545(3) 0.623(2) 0.9757(18) 0.020(8) Uiso 1 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'
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
_geom_angle_publ_flag
N32 Cu1 N5 171.17(13) . . ?
N32 Cu1 N1 99.54(13) . . ?
N5 Cu1 N1 80.32(11) . . ?
N32 Cu1 N2 99.30(13) . . ?
N5 Cu1 N2 80.02(11) . . ?
N1 Cu1 N2 159.99(12) . . ?
N32 Cu1 N36 92.69(14) . . ?
N5 Cu1 N36 96.10(11) . . ?
N1 Cu1 N36 96.37(11) . . ?
N2 Cu1 N36 89.42(11) . . ?
N40 Cu2 N6 162.12(13) . . ?
N40 Cu2 N3 98.99(13) . . ?
N6 Cu2 N3 80.57(12) . . ?
N40 Cu2 N4 98.31(13) . . ?
N6 Cu2 N4 80.07(12) . . ?
N3 Cu2 N4 160.31(13) . . ?
N40 Cu2 N44 98.15(14) . . ?
N6 Cu2 N44 99.68(13) . . ?
N3 Cu2 N44 96.19(14) . . ?
N4 Cu2 N44 90.57(13) . . ?
C1 N1 C5 119.0(3) . . ?
C1 N1 Cu1 124.7(3) . . ?
C5 N1 Cu1 115.2(2) . . ?
C10 N2 C6 118.9(3) . . ?
C10 N2 Cu1 124.8(3) . . ?
C6 N2 Cu1 114.5(2) . . ?
C16 N4 C20 119.1(3) . . ?
C16 N4 Cu2 124.6(3) . . ?
C20 N4 Cu2 114.7(2) . . ?
C15 N3 C11 118.7(4) . . ?
C15 N3 Cu2 125.4(3) . . ?
C11 N3 Cu2 114.6(2) . . ?
C24 N5 C21 125.2(3) . . ?
C24 N5 Cu1 117.8(2) . . ?
C21 N5 Cu1 117.1(2) . . ?
C22 N6 C23 125.4(3) . . ?
C22 N6 Cu2 116.9(2) . . ?
C23 N6 Cu2 117.7(2) . . ?
N1 C1 C2 122.1(4) . . ?
C3 C2 C1 119.4(5) . . ?
C2 C3 C4 119.3(5) . . ?
C5 C4 C3 119.0(4) . . ?
N1 C5 C4 121.0(3) . . ?
N1 C5 C21 113.2(3) . . ?
C4 C5 C21 125.5(3) . . ?
N2 C6 C7 121.4(3) . . ?
N2 C6 C24 113.6(3) . . ?
C7 C6 C24 125.0(3) . . ?
C6 C7 C8 118.4(4) . . ?
C9 C8 C7 120.3(4) . . ?
C8 C9 C10 119.0(4) . . ?
N2 C10 C9 121.8(4) . . ?
N3 C11 C12 121.2(3) . . ?
N3 C11 C22 113.4(3) . . ?
C12 C11 C22 125.1(4) . . ?
C11 C12 C13 118.6(5) . . ?
C14 C13 C12 119.9(5) . . ?
C13 C14 C15 118.7(4) . . ?
N3 C15 C14 122.7(5) . . ?
N4 C16 C17 122.5(4) . . ?
C18 C17 C16 118.9(4) . . ?
C17 C18 C19 119.5(4) . . ?
C18 C19 C20 119.7(4) . . ?
N4 C20 C19 120.2(3) . . ?
N4 C20 C23 113.5(3) . . ?
C19 C20 C23 126.1(3) . . ?
N5 C21 C22 116.1(3) . . ?
N5 C21 C5 112.9(3) . . ?
C22 C21 C5 131.0(3) . . ?
N6 C22 C21 116.8(3) . . ?
N6 C22 C11 112.6(3) . . ?
C21 C22 C11 130.6(3) . . ?
N6 C23 C24 116.3(3) . . ?
N6 C23 C20 112.8(3) . . ?
C24 C23 C20 130.9(3) . . ?
N5 C24 C23 116.9(3) . . ?
N5 C24 C6 112.1(3) . . ?
C23 C24 C6 130.9(3) . . ?
C32 N32 Cu1 176.8(4) . . ?
C32 C31 C34 118.3(5) . . ?
C32 C31 C33 117.9(4) . . ?
C34 C31 C33 123.8(4) . . ?
N32 C32 C31 179.8(6) . . ?
N33 C33 C31 177.2(6) . . ?
N34 C34 C31 177.9(7) . . ?
C36 N36 Cu1 172.2(3) . . ?
C36 C35 C37 120.1(3) . . ?
C36 C35 C38 120.3(3) . . ?
C37 C35 C38 119.6(3) . . ?
N36 C36 C35 179.0(4) . . ?
N37 C37 C35 178.9(5) . . ?
N38 C38 C35 178.4(4) . . ?
C40 N40 Cu2 168.5(3) . . ?
C40 C39 C42 118.3(4) . . ?
C40 C39 C41 118.9(3) . . ?
C42 C39 C41 122.8(3) . . ?
N40 C40 C39 177.9(4) . . ?
N41 C41 C39 177.4(5) . . ?
N42 C42 C39 179.1(4) . . ?
C44 N44 Cu2 173.4(3) . . ?
C44 C43 C45 117.6(4) . . ?
C44 C43 C46 120.7(4) . . ?
C45 C43 C46 121.2(4) . . ?
N44 C44 C43 179.0(4) . . ?
N45 C45 C43 178.6(5) . . ?
N46 C46 C43 179.4(5) . . ?
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
Cu1 N32 1.944(3) . ?
Cu1 N5 1.962(3) . ?
Cu1 N1 2.000(3) . ?
Cu1 N2 2.006(3) . ?
Cu1 N36 2.308(4) . ?
Cu2 N40 1.949(3) . ?
Cu2 N6 1.961(3) . ?
Cu2 N3 1.994(3) . ?
Cu2 N4 2.004(3) . ?
Cu2 N44 2.175(4) . ?
N1 C1 1.334(5) . ?
N1 C5 1.358(4) . ?
N2 C10 1.348(4) . ?
N2 C6 1.349(4) . ?
N4 C16 1.329(5) . ?
N4 C20 1.359(4) . ?
N3 C15 1.342(5) . ?
N3 C11 1.353(5) . ?
N5 C24 1.337(4) . ?
N5 C21 1.346(4) . ?
N6 C22 1.337(4) . ?
N6 C23 1.340(4) . ?
C1 C2 1.369(6) . ?
C2 C3 1.359(7) . ?
C3 C4 1.390(6) . ?
C4 C5 1.368(5) . ?
C5 C21 1.481(5) . ?
C6 C7 1.381(5) . ?
C6 C24 1.486(4) . ?
C7 C8 1.389(5) . ?
C8 C9 1.349(7) . ?
C9 C10 1.380(6) . ?
C11 C12 1.379(5) . ?
C11 C22 1.483(4) . ?
C12 C13 1.390(6) . ?
C13 C14 1.365(7) . ?
C14 C15 1.367(7) . ?
C16 C17 1.373(6) . ?
C17 C18 1.363(6) . ?
C18 C19 1.374(5) . ?
C19 C20 1.380(5) . ?
C20 C23 1.478(5) . ?
C21 C22 1.407(4) . ?
C23 C24 1.404(4) . ?
N32 C32 1.136(5) . ?
N33 C33 1.143(7) . ?
N34 C34 1.139(7) . ?
C31 C32 1.394(5) . ?
C31 C34 1.406(8) . ?
C31 C33 1.411(8) . ?
N36 C36 1.144(4) . ?
N37 C37 1.142(4) . ?
N38 C38 1.148(4) . ?
C35 C36 1.400(5) . ?
C35 C37 1.409(5) . ?
C35 C38 1.410(5) . ?
N40 C40 1.145(4) . ?
N42 C42 1.139(5) . ?
N41 C41 1.141(5) . ?
C39 C40 1.382(5) . ?
C39 C42 1.405(5) . ?
C39 C41 1.408(6) . ?
N44 C44 1.142(5) . ?
N46 C46 1.131(6) . ?
N45 C45 1.157(6) . ?
C43 C44 1.395(6) . ?
C43 C45 1.401(8) . ?
C43 C46 1.412(8) . ?
