#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:52:31 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179351 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/48/4324888.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_4324888
loop_
_publ_author_name
'Sandip Mukherjee'
'Bappaditya Gole'
'You Song'
'Partha Sarathi Mukherjee'
_publ_section_title
;
 Synthesis, Structures, and Magnetic Behavior of a Series of Copper(II)
 Azide Polymers of Cu4 Building Clusters and Isolation of a New Hemiaminal
 Ether as the Metal Complex
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3621
_journal_page_last               3631
_journal_paper_doi               10.1021/ic102580a
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C12 H19 Cu2 N15'
_chemical_formula_sum            'C12 H19 Cu2 N15'
_chemical_formula_weight         500.50
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.199(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.0755(10)
_cell_length_b                   11.1386(8)
_cell_length_c                   16.5852(14)
_cell_measurement_reflns_used    6045
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.50
_cell_measurement_theta_min      2.00
_cell_volume                     1992.0(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1999)'
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0726
_diffrn_reflns_av_sigmaI/netI    0.0837
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            34974
_diffrn_reflns_theta_full        30.55
_diffrn_reflns_theta_max         30.55
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    2.169
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6576
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.669
_exptl_crystal_description       rod
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.808
_refine_diff_density_min         -0.703
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         6045
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.1148
_refine_ls_R_factor_gt           0.0477
_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)+(0.0438P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0921
_refine_ls_wR_factor_ref         0.1099
_reflns_number_gt                3327
_reflns_number_total             6045
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ic102580a_si_002_3.cif
_cod_data_source_block           complex3
_cod_database_code               4324888
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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
Cu1 Cu 0.84852(3) 0.12179(3) 0.24007(2) 0.03020(12) Uani 1 1 d .
Cu2 Cu 0.99709(3) -0.03828(3) 0.40699(2) 0.03953(13) Uani 1 1 d .
N3 N 0.9648(2) 0.0729(2) 0.15991(14) 0.0305(6) Uani 1 1 d .
N2 N 0.7157(2) 0.0868(2) 0.14346(16) 0.0345(6) Uani 1 1 d .
N1 N 0.6922(2) 0.1341(2) 0.29116(17) 0.0373(6) Uani 1 1 d .
C4 C 0.4721(3) 0.1018(3) 0.2555(3) 0.0589(11) Uani 1 1 d .
H4 H 0.4006 0.0842 0.2155 0.071 Uiso 1 1 calc R
C9 C 1.0691(3) -0.0069(3) 0.2024(2) 0.0392(8) Uani 1 1 d .
H9A H 1.0341 -0.0740 0.2265 0.047 Uiso 1 1 calc R
H9B H 1.1207 0.0379 0.2476 0.047 Uiso 1 1 calc R
C5 C 0.5856(3) 0.1080(3) 0.2354(2) 0.0413(8) Uani 1 1 d .
C8 C 0.8805(3) 0.0029(3) 0.09287(19) 0.0401(8) Uani 1 1 d .
H8A H 0.8703 -0.0776 0.1125 0.048 Uiso 1 1 calc R
H8B H 0.9176 -0.0034 0.0454 0.048 Uiso 1 1 calc R
C1 C 0.6846(3) 0.1547(3) 0.3691(2) 0.0498(9) Uani 1 1 d .
H1 H 0.7566 0.1731 0.4084 0.060 Uiso 1 1 calc R
C12 C 1.1032(3) 0.2571(3) 0.1830(2) 0.0587(10) Uani 1 1 d .
H12A H 1.1282 0.3246 0.1547 0.088 Uiso 1 1 calc R
H12B H 1.1746 0.2095 0.2071 0.088 Uiso 1 1 calc R
H12C H 1.0649 0.2851 0.2259 0.088 Uiso 1 1 calc R
C11 C 1.0118(3) 0.1817(3) 0.1222(2) 0.0417(8) Uani 1 1 d .
H11A H 0.9415 0.2315 0.0968 0.050 Uiso 1 1 calc R
H11B H 1.0510 0.1552 0.0786 0.050 Uiso 1 1 calc R
N11 N 1.1611(3) -0.2350(3) 0.4213(2) 0.0600(9) Uani 1 1 d .
C6 C 0.6051(3) 0.0843(3) 0.1517(2) 0.0440(8) Uani 1 1 d .
H6 H 0.5391 0.0683 0.1072 0.053 Uiso 1 1 calc R
C7 C 0.7541(3) 0.0630(3) 0.06671(19) 0.0441(8) Uani 1 1 d .
H7A H 0.7601 0.1372 0.0372 0.053 Uiso 1 1 calc R
H7B H 0.6953 0.0104 0.0311 0.053 Uiso 1 1 calc R
C10 C 1.1522(3) -0.0567(3) 0.1482(2) 0.0516(9) Uani 1 1 d .
H10A H 1.2151 -0.1068 0.1811 0.077 Uiso 1 1 calc R
H10B H 1.1905 0.0085 0.1256 0.077 Uiso 1 1 calc R
H10C H 1.1030 -0.1032 0.1039 0.077 Uiso 1 1 calc R
C3 C 0.4674(4) 0.1225(4) 0.3370(3) 0.0694(12) Uani 1 1 d .
H3 H 0.3923 0.1180 0.3529 0.083 Uiso 1 1 calc R
N10 N 1.1239(4) -0.1483(4) 0.3824(3) 0.1123(17) Uani 1 1 d .
N12 N 1.2074(4) -0.3154(3) 0.4519(2) 0.0831(12) Uani 1 1 d .
N4 N 0.9744(2) 0.1375(2) 0.34379(15) 0.0375(6) Uani 1 1 d .
N8 N 0.7686(3) -0.1318(2) 0.30187(16) 0.0367(6) Uani 1 1 d .
N5 N 0.9994(3) 0.2318(3) 0.37949(18) 0.0487(7) Uani 1 1 d .
N7 N 0.8696(3) -0.0912(3) 0.30747(19) 0.0567(8) Uani 1 1 d .
C2 C 0.5736(4) 0.1496(3) 0.3937(3) 0.0670(12) Uani 1 1 d .
H2 H 0.5714 0.1644 0.4485 0.080 Uiso 1 1 calc R
N9 N 0.6701(3) -0.1691(2) 0.29060(19) 0.0500(8) Uani 1 1 d .
N6 N 1.0255(4) 0.3202(3) 0.4132(3) 0.1016(15) Uani 1 1 d .
N13 N 1.1157(2) 0.0296(3) 0.50507(17) 0.0502(8) Uani 1 1 d .
N14 N 1.2116(3) 0.0751(3) 0.49867(17) 0.0480(7) Uani 1 1 d .
N15 N 1.3019(3) 0.1173(3) 0.4917(2) 0.0856(13) Uani 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'
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
N2 Cu1 N4 172.24(10) . .
N2 Cu1 N1 78.92(10) . .
N4 Cu1 N1 97.30(11) . .
N2 Cu1 N3 83.46(10) . .
N4 Cu1 N3 99.24(10) . .
N1 Cu1 N3 160.79(10) . .
N2 Cu1 N9 90.43(10) . 2_655
N4 Cu1 N9 96.31(10) . 2_655
N1 Cu1 N9 89.03(10) . 2_655
N3 Cu1 N9 98.76(10) . 2_655
N10 Cu2 N13 92.11(16) . .
N10 Cu2 N7 92.77(16) . .
N13 Cu2 N7 174.46(12) . .
N10 Cu2 N13 136.54(16) . 3_756
N13 Cu2 N13 78.71(12) . 3_756
N7 Cu2 N13 99.47(12) . 3_756
N10 Cu2 N4 117.46(16) . .
N13 Cu2 N4 91.91(11) . .
N7 Cu2 N4 83.51(11) . .
N13 Cu2 N4 105.33(11) 3_756 .
C8 N3 C9 108.9(2) . .
C8 N3 C11 109.0(2) . .
C9 N3 C11 111.7(2) . .
C8 N3 Cu1 103.52(17) . .
C9 N3 Cu1 111.71(18) . .
C11 N3 Cu1 111.70(18) . .
C6 N2 C7 125.1(3) . .
C6 N2 Cu1 118.9(2) . .
C7 N2 Cu1 116.01(19) . .
C1 N1 C5 117.4(3) . .
C1 N1 Cu1 130.0(2) . .
C5 N1 Cu1 112.4(2) . .
C5 C4 C3 118.0(4) . .
C5 C4 H4 121.0 . .
C3 C4 H4 121.0 . .
N3 C9 C10 116.2(3) . .
N3 C9 H9A 108.2 . .
C10 C9 H9A 108.2 . .
N3 C9 H9B 108.2 . .
C10 C9 H9B 108.2 . .
H9A C9 H9B 107.4 . .
N1 C5 C4 123.3(4) . .
N1 C5 C6 112.9(3) . .
C4 C5 C6 123.9(3) . .
N3 C8 C7 111.1(2) . .
N3 C8 H8A 109.4 . .
C7 C8 H8A 109.4 . .
N3 C8 H8B 109.4 . .
C7 C8 H8B 109.4 . .
H8A C8 H8B 108.0 . .
N1 C1 C2 122.4(4) . .
N1 C1 H1 118.8 . .
C2 C1 H1 118.8 . .
C11 C12 H12A 109.5 . .
C11 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C11 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
N3 C11 C12 114.3(3) . .
N3 C11 H11A 108.7 . .
C12 C11 H11A 108.7 . .
N3 C11 H11B 108.7 . .
C12 C11 H11B 108.7 . .
H11A C11 H11B 107.6 . .
N12 N11 N10 170.9(5) . .
N2 C6 C5 116.9(3) . .
N2 C6 H6 121.6 . .
C5 C6 H6 121.6 . .
N2 C7 C8 105.3(2) . .
N2 C7 H7A 110.7 . .
C8 C7 H7A 110.7 . .
N2 C7 H7B 110.7 . .
C8 C7 H7B 110.7 . .
H7A C7 H7B 108.8 . .
C9 C10 H10A 109.5 . .
C9 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C9 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
C2 C3 C4 119.5(4) . .
C2 C3 H3 120.2 . .
C4 C3 H3 120.2 . .
N11 N10 Cu2 124.8(4) . .
N5 N4 Cu1 123.1(2) . .
N5 N4 Cu2 123.4(2) . .
Cu1 N4 Cu2 108.60(11) . .
N9 N8 N7 175.1(4) . .
N6 N5 N4 178.5(4) . .
N8 N7 Cu2 130.5(3) . .
C3 C2 C1 119.5(4) . .
C3 C2 H2 120.3 . .
C1 C2 H2 120.3 . .
N8 N9 Cu1 115.1(2) . 2_645
N14 N13 Cu2 121.2(2) . .
N14 N13 Cu2 135.2(2) . 3_756
Cu2 N13 Cu2 101.29(12) . 3_756
N15 N14 N13 179.1(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N2 1.951(2) .
Cu1 N4 1.959(2) .
Cu1 N1 2.098(3) .
Cu1 N3 2.123(2) .
Cu1 N9 2.383(3) 2_655
Cu2 N10 1.975(4) .
Cu2 N13 1.992(3) .
Cu2 N7 2.000(3) .
Cu2 N13 2.128(3) 3_756
Cu2 N4 2.208(2) .
N3 C8 1.497(4) .
N3 C9 1.499(4) .
N3 C11 1.510(4) .
N2 C6 1.263(4) .
N2 C7 1.455(4) .
N1 C1 1.335(4) .
N1 C5 1.355(4) .
C4 C5 1.374(5) .
C4 C3 1.385(6) .
C4 H4 0.9300 .
C9 C10 1.530(4) .
C9 H9A 0.9700 .
C9 H9B 0.9700 .
C5 C6 1.476(5) .
C8 C7 1.523(4) .
C8 H8A 0.9700 .
C8 H8B 0.9700 .
C1 C2 1.382(5) .
C1 H1 0.9300 .
C12 C11 1.511(5) .
C12 H12A 0.9600 .
C12 H12B 0.9600 .
C12 H12C 0.9600 .
C11 H11A 0.9700 .
C11 H11B 0.9700 .
N11 N12 1.097(4) .
N11 N10 1.183(5) .
C6 H6 0.9300 .
C7 H7A 0.9700 .
C7 H7B 0.9700 .
C10 H10A 0.9600 .
C10 H10B 0.9600 .
C10 H10C 0.9600 .
C3 C2 1.361(6) .
C3 H3 0.9300 .
N4 N5 1.206(3) .
N8 N9 1.142(3) .
N8 N7 1.191(4) .
N5 N6 1.137(4) .
C2 H2 0.9300 .
N9 Cu1 2.383(3) 2_645
N13 N14 1.202(4) .
N13 Cu2 2.128(3) 3_756
N14 N15 1.135(4) .
