#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/26/2202690.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_2202690
loop_
_publ_author_name
'Qihua Zhao'
'Xiaofeng Wang'
'Ruibin Fang'
'Tiekink, Edward R. T.'
_publ_section_title
;
 Di-μ-azido-bis[azido(4,7-dimethyl-1,10-phenanthroline)copper(II)]
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m722
_journal_page_last               m723
_journal_paper_doi               10.1107/S1600536803015861
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '[Cu2 (N3)4 (C14 H12 N2)2]'
_chemical_formula_moiety         'C28 H24 Cu2 N16'
_chemical_formula_sum            'C28 H24 Cu2 N16'
_chemical_formula_weight         711.72
_chemical_name_systematic        ?
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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
_cell_angle_beta                 95.565(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3691(5)
_cell_length_b                   11.2648(5)
_cell_length_c                   19.5792(9)
_cell_measurement_reflns_used    3661
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      30.0
_cell_measurement_theta_min      2.4
_cell_volume                     2934.7(2)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SHELXTL (Bruker, 2000)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHEXLTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'PATTY in DIRDIF92 (Beurskens et al., 1992)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker AXS SMART CCD'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.032
_diffrn_reflns_av_sigmaI/netI    0.041
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            11979
_diffrn_reflns_theta_full        30.0
_diffrn_reflns_theta_max         30.0
_diffrn_reflns_theta_min         2.1
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.501
_exptl_absorpt_correction_T_max  0.787
_exptl_absorpt_correction_T_min  0.750
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000; Blessing, 1995)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.611
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.62
_refine_diff_density_min         -0.33
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.04
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         4259
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.04
_refine_ls_R_factor_all          0.048
_refine_ls_R_factor_gt           0.037
_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)+(0.0584P)²+0.0245P] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.095
_refine_ls_wR_factor_ref         0.101
_reflns_number_gt                3450
_reflns_number_total             4259
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            lh6087.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2202690
_cod_database_fobs_code          2202690
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_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
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Cu 0.152642(16) 0.259903(18) 0.039472(11) 0.02300(9) Uani d . 1 . . Cu
N1 0.30477(13) 0.26186(14) 0.05616(9) 0.0285(3) Uani d . 1 . . N
N2 0.35279(13) 0.23119(15) 0.10891(9) 0.0309(4) Uani d . 1 . . N
N3 0.39785(17) 0.2044(2) 0.15878(10) 0.0558(6) Uani d . 1 . . N
N4 0.01649(13) 0.29821(17) 0.00094(9) 0.0348(4) Uani d . 1 . . N
N5 -0.05016(12) 0.33126(16) 0.03205(8) 0.0327(4) Uani d . 1 . . N
N6 -0.11857(16) 0.3630(2) 0.05827(10) 0.0570(6) Uani d . 1 . . N
N7 0.13577(11) 0.31505(13) 0.13648(7) 0.0233(3) Uani d . 1 . . N
N8 0.13538(11) 0.08577(13) 0.09397(8) 0.0253(3) Uani d . 1 . . N
C1 0.13146(14) 0.42862(16) 0.15577(10) 0.0271(4) Uani d . 1 . . C
C2 0.12784(15) 0.45956(18) 0.22500(11) 0.0331(4) Uani d . 1 . . C
H2 0.1249 0.5399 0.2376 0.040 Uiso calc R 1 . . H
C3 0.12863(15) 0.37389(19) 0.27385(10) 0.0338(4) Uani d . 1 . . C
H3 0.1273 0.3949 0.3202 0.041 Uiso calc R 1 . . H
C4 0.13139(15) 0.25342(16) 0.25485(10) 0.0283(4) Uani d . 1 . . C
C5 0.13421(14) 0.22804(16) 0.18496(10) 0.0236(4) Uani d . 1 . . C
C6 0.13254(13) 0.10597(16) 0.16216(9) 0.0248(4) Uani d . 1 . . C
C7 0.12679(15) 0.01531(18) 0.21068(10) 0.0306(4) Uani d . 1 . . C
C8 0.12536(15) 0.0440(2) 0.28141(11) 0.0372(5) Uani d . 1 . . C
H8 0.1224 -0.0174 0.3137 0.045 Uiso calc R 1 . . H
C9 0.12818(15) 0.1579(2) 0.30287(10) 0.0357(5) Uani d . 1 . . C
H9 0.1280 0.1748 0.3499 0.043 Uiso calc R 1 . . H
C10 0.12010(17) -0.10215(18) 0.18507(11) 0.0388(5) Uani d . 1 . . C
H10 0.1148 -0.1664 0.2151 0.047 Uiso calc R 1 . . H
C11 0.12147(17) -0.12118(18) 0.11668(12) 0.0391(5) Uani d . 1 . . C
H11 0.1159 -0.1990 0.0994 0.047 Uiso calc R 1 . . H
C12 0.13115(14) -0.02539(16) 0.07126(10) 0.0292(4) Uani d . 1 . . C
C13 0.12982(17) 0.52244(17) 0.10197(11) 0.0365(5) Uani d . 1 . . C
H13A 0.1420 0.4866 0.0585 0.055 Uiso calc R 1 . . H
H13B 0.1817 0.5806 0.1149 0.055 Uiso calc R 1 . . H
H13C 0.0647 0.5611 0.0975 0.055 Uiso calc R 1 . . H
C14 0.13416(17) -0.04688(18) -0.00341(11) 0.0372(5) Uani d . 1 . . C
H14A 0.1422 0.0281 -0.0266 0.056 Uiso calc R 1 . . H
H14B 0.0720 -0.0842 -0.0219 0.056 Uiso calc R 1 . . H
H14C 0.1903 -0.0986 -0.0105 0.056 Uiso calc R 1 . . H
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 Cu N4 . . 160.67(7) y
N1 Cu N7 . . 92.67(6) y
N1 Cu N8 . . 94.60(6) y
N1 Cu N1 . 7 77.45(7) y
N4 Cu N7 . . 96.31(7) y
N4 Cu N8 . . 103.95(7) y
N4 Cu N1 . 7 90.27(7) y
N7 Cu N8 . . 78.34(6) y
N7 Cu N1 . 7 165.60(6) y
N8 Cu N1 . 7 112.53(6) y
Cu N1 N2 . . 125.03(14) y
Cu N1 N2 7 . 125.47(14) y
Cu N1 Cu . 7 102.55(7) y
N1 N2 N3 . . 178.8(2) y
Cu N4 N5 . . 126.15(14) y
N4 N5 N6 . . 175.6(2) y
C1 N7 C5 . . 119.11(16) ?
C1 N7 Cu . . 124.64(12) ?
C5 N7 Cu . . 116.16(12) ?
C12 N8 C6 . . 118.85(16) ?
C12 N8 Cu . . 131.65(13) ?
C6 N8 Cu . . 109.46(11) ?
N7 C1 C2 . . 121.09(17) ?
N7 C1 C13 . . 118.49(17) ?
C2 C1 C13 . . 120.42(17) ?
C3 C2 C1 . . 120.31(18) ?
C3 C2 H2 . . 119.8 ?
C1 C2 H2 . . 119.8 ?
C2 C3 C4 . . 119.81(18) ?
C2 C3 H3 . . 120.1 ?
C4 C3 H3 . . 120.1 ?
C5 C4 C3 . . 117.27(17) ?
C5 C4 C9 . . 119.53(17) ?
C3 C4 C9 . . 123.16(18) ?
N7 C5 C4 . . 122.38(16) ?
N7 C5 C6 . . 117.96(16) ?
C4 C5 C6 . . 119.64(16) ?
N8 C6 C7 . . 123.54(17) ?
N8 C6 C5 . . 117.51(15) ?
C7 C6 C5 . . 118.94(17) ?
C6 C7 C10 . . 116.54(18) ?
C6 C7 C8 . . 120.03(18) ?
C10 C7 C8 . . 123.41(18) ?
C9 C8 C7 . . 121.06(19) ?
C9 C8 H8 . . 119.5 ?
C7 C8 H8 . . 119.5 ?
C8 C9 C4 . . 120.76(18) ?
C8 C9 H9 . . 119.6 ?
C4 C9 H9 . . 119.6 ?
C11 C10 C7 . . 119.39(18) ?
C11 C10 H10 . . 120.3 ?
C7 C10 H10 . . 120.3 ?
C10 C11 C12 . . 120.74(19) ?
C10 C11 H11 . . 119.6 ?
C12 C11 H11 . . 119.6 ?
N8 C12 C11 . . 120.88(18) ?
N8 C12 C14 . . 118.58(17) ?
C11 C12 C14 . . 120.52(17) ?
C1 C13 H13A . . 109.5 ?
C1 C13 H13B . . 109.5 ?
H13A C13 H13B . . 109.5 ?
C1 C13 H13C . . 109.5 ?
H13A C13 H13C . . 109.5 ?
H13B C13 H13C . . 109.5 ?
C12 C14 H14A . . 109.5 ?
C12 C14 H14B . . 109.5 ?
H14A C14 H14B . . 109.5 ?
C12 C14 H14C . . 109.5 ?
H14A C14 H14C . . 109.5 ?
H14B C14 H14C . . 109.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cu N1 . 2.0285(17) y
Cu N4 . 1.9499(17) y
Cu N7 . 2.0316(15) y
Cu N8 . 2.2554(15) y
Cu N1 7 2.0240(17) y
N1 N2 . 1.212(2) y
N2 N3 . 1.137(2) y
N4 N5 . 1.187(2) y
N5 N6 . 1.149(2) y
N7 C1 . 1.337(2) ?
N7 C5 . 1.366(2) ?
N8 C12 . 1.328(2) ?
N8 C6 . 1.359(2) ?
C1 C2 . 1.405(3) ?
C1 C13 . 1.491(3) ?
C2 C3 . 1.358(3) ?
C2 H2 . 0.9400 ?
C3 C4 . 1.409(3) ?
C3 H3 . 0.9400 ?
C4 C5 . 1.402(3) ?
C4 C9 . 1.432(3) ?
C5 C6 . 1.445(3) ?
C6 C7 . 1.402(2) ?
C7 C10 . 1.415(3) ?
C7 C8 . 1.424(3) ?
C8 C9 . 1.350(3) ?
C8 H8 . 0.9400 ?
C9 H9 . 0.9400 ?
C10 C11 . 1.358(3) ?
C10 H10 . 0.9400 ?
C11 C12 . 1.412(3) ?
C11 H11 . 0.9400 ?
C12 C14 . 1.486(3) ?
C13 H13A . 0.9700 ?
C13 H13B . 0.9700 ?
C13 H13C . 0.9700 ?
C14 H14A . 0.9700 ?
C14 H14B . 0.9700 ?
C14 H14C . 0.9700 ?
