#------------------------------------------------------------------------------
#$Date: 2016-03-25 09:04:38 +0100 (vie 25 de mar de 2016) $
#$Revision: 179739 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/35/7003583.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_7003583
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            'C16 H7 Cu N9'
_chemical_formula_weight         388.84
_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
_cell_angle_alpha                116.319(4)
_cell_angle_beta                 90.635(4)
_cell_angle_gamma                108.260(4)
_cell_formula_units_Z            2
_cell_length_a                   7.4889(4)
_cell_length_b                   11.0496(5)
_cell_length_c                   11.5924(5)
_cell_measurement_temperature    293(2)
_cell_volume                     803.75(8)
_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 0.975
_diffrn_measured_fraction_theta_max 0.975
_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  0.0147
_diffrn_reflns_av_sigmaI/netI    0.0215
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7681
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         5.30
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    1.380
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             390
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.441
_refine_diff_density_min         -0.433
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         3599
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0268
_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)+(0.0311P)²+0.4532P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0675
_refine_ls_wR_factor_ref         0.0697
_reflns_number_gt                3324
_reflns_number_total             3599
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b717347d.txt
_cod_data_source_block           ull1350b
_cod_original_cell_volume        803.75(7)
_cod_database_code               7003583
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 0.42695(3) 0.35207(2) 0.742574(19) 0.02553(8) Uani 1 1 d . . .
N1 N 0.3356(2) 0.13783(16) 0.61227(14) 0.0272(3) Uani 1 1 d . . .
N2 N 0.3112(2) 0.35686(17) 0.59090(15) 0.0322(3) Uani 1 1 d . . .
C4 C 0.1713(3) -0.0387(2) 0.39571(19) 0.0349(4) Uani 1 1 d . . .
N11 N 0.6143(2) 0.32983(18) 0.84801(15) 0.0336(3) Uani 1 1 d . . .
N12 N 1.1908(2) 0.33344(18) 0.85129(16) 0.0343(3) Uani 1 1 d . . .
N13 N 0.9104(5) 0.3396(5) 1.1874(3) 0.1251(16) Uani 1 1 d . . .
N14 N 0.5454(3) 0.56340(18) 0.83649(17) 0.0433(4) Uani 1 1 d . . .
N15 N 0.9217(3) 0.9940(2) 1.14833(18) 0.0468(5) Uani 1 1 d . . .
N16 N 0.5622(4) 0.9471(3) 0.8137(3) 0.0690(7) Uani 1 1 d . . .
C1 C 0.3486(3) 0.0327(2) 0.6362(2) 0.0334(4) Uani 1 1 d . . .
C2 C 0.2733(3) -0.1110(2) 0.5431(2) 0.0387(4) Uani 1 1 d . . .
C3 C 0.1831(3) -0.1468(2) 0.4221(2) 0.0389(4) Uani 1 1 d . . .
C5 C 0.2482(2) 0.10225(19) 0.49333(17) 0.0278(4) Uani 1 1 d . . .
C6 C 0.2396(3) 0.2280(2) 0.48590(17) 0.0292(4) Uani 1 1 d . . .
N3 N 0.1592(3) 0.2385(2) 0.38864(17) 0.0374(4) Uani 1 1 d . . .
C7 C 0.1783(4) 0.3788(3) 0.4330(2) 0.0469(5) Uani 1 1 d . . .
C8 C 0.2738(4) 0.4523(2) 0.5585(2) 0.0442(5) Uani 1 1 d . . .
C11 C 0.8993(3) 0.3243(2) 0.96259(18) 0.0292(4) Uani 1 1 d . . .
C12 C 0.7402(2) 0.32690(18) 0.90176(17) 0.0265(3) Uani 1 1 d . . .
C13 C 1.0609(3) 0.32915(18) 0.90279(17) 0.0268(4) Uani 1 1 d . . .
C14 C 0.9039(4) 0.3315(4) 1.0861(2) 0.0590(7) Uani 1 1 d . . .
C16 C 0.6053(3) 0.6870(2) 0.88469(18) 0.0322(4) Uani 1 1 d . . .
C15 C 0.6745(3) 0.83628(19) 0.93894(18) 0.0323(4) Uani 1 1 d . . .
C17 C 0.8104(3) 0.9228(2) 1.05446(19) 0.0329(4) Uani 1 1 d . . .
C18 C 0.6121(3) 0.8993(2) 0.8713(2) 0.0401(5) Uani 1 1 d . . .
H1 H 0.406(3) 0.060(2) 0.719(2) 0.042(6) Uiso 1 1 d . . .
H8 H 0.319(3) 0.548(3) 0.617(2) 0.036(6) Uiso 1 1 d . . .
H4 H 0.120(3) -0.057(2) 0.318(2) 0.040(6) Uiso 1 1 d . . .
H7 H 0.137(3) 0.411(2) 0.382(2) 0.042(6) Uiso 1 1 d . . .
H2 H 0.283(4) -0.185(3) 0.568(3) 0.055(7) Uiso 1 1 d . . .
H5 H 0.095(4) 0.169(3) 0.316(3) 0.050(7) Uiso 1 1 d . . .
H3 H 0.135(3) -0.242(3) 0.358(2) 0.047(7) 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 0.0030 0.0020 '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'
Cu Cu 0.3200 1.2650 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0060 0.0030 '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
N14 Cu1 N2 91.73(7) . . ?
N14 Cu1 N11 91.95(7) . . ?
N2 Cu1 N11 157.68(7) . . ?
N14 Cu1 N1 166.88(7) . . ?
N2 Cu1 N1 80.67(6) . . ?
N11 Cu1 N1 91.21(6) . . ?
N14 Cu1 N12 96.97(8) . 1_455 ?
N2 Cu1 N12 102.40(7) . 1_455 ?
N11 Cu1 N12 99.00(6) . 1_455 ?
N1 Cu1 N12 95.11(6) . 1_455 ?
C1 N1 C5 118.91(16) . . ?
C1 N1 Cu1 126.08(13) . . ?
C5 N1 Cu1 114.95(12) . . ?
C6 N2 C8 106.53(16) . . ?
C6 N2 Cu1 113.45(12) . . ?
C8 N2 Cu1 139.98(14) . . ?
C5 C4 C3 118.34(19) . . ?
C12 N11 Cu1 170.56(16) . . ?
C13 N12 Cu1 173.92(15) . 1_655 ?
C16 N14 Cu1 174.79(16) . . ?
N1 C1 C2 121.85(19) . . ?
C3 C2 C1 119.00(19) . . ?
C2 C3 C4 119.64(19) . . ?
N1 C5 C4 122.25(18) . . ?
N1 C5 C6 111.72(15) . . ?
C4 C5 C6 125.98(17) . . ?
N2 C6 N3 110.28(17) . . ?
N2 C6 C5 119.20(16) . . ?
N3 C6 C5 130.43(17) . . ?
C6 N3 C7 107.78(17) . . ?
N3 C7 C8 106.80(19) . . ?
C7 C8 N2 108.61(19) . . ?
C12 C11 C14 120.71(18) . . ?
C12 C11 C13 118.05(16) . . ?
C14 C11 C13 120.93(17) . . ?
N11 C12 C11 177.1(2) . . ?
N12 C13 C11 178.17(19) . . ?
N13 C14 C11 178.8(4) . . ?
N14 C16 C15 177.9(2) . . ?
C16 C15 C17 121.10(17) . . ?
C16 C15 C18 118.28(17) . . ?
C17 C15 C18 120.54(17) . . ?
N15 C17 C15 179.5(2) . . ?
N16 C18 C15 178.1(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
Cu1 N14 1.9624(17) . ?
Cu1 N2 1.9808(15) . ?
Cu1 N11 1.9917(16) . ?
Cu1 N1 2.0359(15) . ?
Cu1 N12 2.1931(17) 1_455 ?
N1 C1 1.339(2) . ?
N1 C5 1.350(2) . ?
N2 C6 1.329(2) . ?
N2 C8 1.365(3) . ?
C4 C5 1.378(3) . ?
C4 C3 1.385(3) . ?
N11 C12 1.141(2) . ?
N12 C13 1.146(2) . ?
N12 Cu1 2.1931(17) 1_655 ?
N13 C14 1.137(3) . ?
N14 C16 1.146(2) . ?
N15 C17 1.144(3) . ?
N16 C18 1.138(3) . ?
C1 C2 1.381(3) . ?
C2 C3 1.378(3) . ?
C5 C6 1.450(3) . ?
C6 N3 1.339(2) . ?
N3 C7 1.357(3) . ?
C7 C8 1.361(3) . ?
C11 C12 1.392(2) . ?
C11 C14 1.398(3) . ?
C11 C13 1.400(3) . ?
C16 C15 1.386(3) . ?
C15 C17 1.403(3) . ?
C15 C18 1.413(3) . ?
