#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:52:31 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179351 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/48/4324886.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_4324886
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         'C15 H19 Cu2 N15 O'
_chemical_formula_sum            'C15 H19 Cu2 N15 O'
_chemical_formula_weight         552.53
_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                106.620(3)
_cell_angle_beta                 108.265(3)
_cell_angle_gamma                90.265(3)
_cell_formula_units_Z            2
_cell_length_a                   9.9271(16)
_cell_length_b                   10.6663(18)
_cell_length_c                   11.4566(19)
_cell_measurement_reflns_used    5101
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.22
_cell_measurement_theta_min      2.22
_cell_volume                     1097.9(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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0417
_diffrn_reflns_av_sigmaI/netI    0.0621
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12673
_diffrn_reflns_theta_full        27.70
_diffrn_reflns_theta_max         27.7
_diffrn_reflns_theta_min         1.96
_exptl_absorpt_coefficient_mu    1.980
_exptl_absorpt_correction_T_max  0.6479
_exptl_absorpt_correction_T_min  0.4710
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.671
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.870
_refine_diff_density_min         -0.774
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         5101
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1019
_refine_ls_R_factor_gt           0.0599
_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)+(0.0748P)²+0.3052P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1332
_refine_ls_wR_factor_ref         0.1536
_reflns_number_gt                3330
_reflns_number_total             5101
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ic102580a_si_002_1.cif
_cod_data_source_block           complex1
_cod_database_code               4324886
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
Cu1 Cu 0.03558(5) 0.70248(5) 0.23452(5) 0.04200(19) Uani 1 1 d .
Cu2 Cu -0.40007(6) 0.55479(5) 0.14291(5) 0.04409(19) Uani 1 1 d .
N1 N -0.0279(4) 0.8517(4) 0.1679(4) 0.0461(9) Uani 1 1 d .
N2 N 0.2160(4) 0.8375(4) 0.3449(4) 0.0444(9) Uani 1 1 d .
N3 N 0.1224(4) 0.5645(4) 0.3083(3) 0.0403(8) Uani 1 1 d .
N4 N -0.1424(4) 0.5825(4) 0.1173(4) 0.0460(9) Uani 1 1 d .
N5 N -0.1285(4) 0.4758(4) 0.0547(4) 0.0404(8) Uani 1 1 d .
N6 N -0.1208(5) 0.3710(4) -0.0060(4) 0.0653(12) Uani 1 1 d .
N7 N -0.1073(5) 0.7765(4) 0.3911(4) 0.0576(11) Uani 1 1 d .
N8 N -0.2264(5) 0.7575(4) 0.3280(4) 0.0460(9) Uani 1 1 d .
N9 N -0.3489(4) 0.7378(4) 0.2599(4) 0.0539(10) Uani 1 1 d .
N10 N -0.3238(6) 0.4860(5) 0.2847(5) 0.0820(16) Uani 1 1 d .
N11 N -0.3231(5) 0.3869(5) 0.3034(4) 0.0599(12) Uani 1 1 d .
N12 N -0.3179(10) 0.2960(7) 0.3321(7) 0.149(4) Uani 1 1 d .
N13 N -0.5207(5) 0.6124(4) -0.0052(4) 0.0614(12) Uani 1 1 d .
N14 N -0.5325(5) 0.7211(5) -0.0093(4) 0.0656(13) Uani 1 1 d .
N15 N -0.5408(8) 0.8241(5) -0.0136(7) 0.130(3) Uani 1 1 d .
C1 C -0.1648(6) 0.8692(5) 0.1137(5) 0.0613(14) Uani 1 1 d .
H1 H -0.2355 0.8006 0.0905 0.074 Uiso 1 1 calc R
C2 C -0.2024(7) 0.9865(6) 0.0917(6) 0.0772(18) Uani 1 1 d .
H2 H -0.2977 0.9989 0.0570 0.093 Uiso 1 1 calc R
C3 C -0.0958(8) 1.0853(6) 0.1225(7) 0.085(2) Uani 1 1 d .
H3 H -0.1187 1.1653 0.1083 0.103 Uiso 1 1 calc R
C4 C 0.0442(7) 1.0656(5) 0.1739(6) 0.0730(17) Uani 1 1 d .
H4 H 0.1171 1.1308 0.1930 0.088 Uiso 1 1 calc R
C5 C 0.0742(6) 0.9479(5) 0.1967(5) 0.0522(12) Uani 1 1 d .
C6 C 0.2235(5) 0.9125(5) 0.2552(5) 0.0542(13) Uani 1 1 d .
H6 H 0.2548 0.8566 0.1863 0.065 Uiso 1 1 calc R
C7 C 0.4507(14) 1.0318(8) 0.2572(8) 0.194(7) Uani 1 1 d .
H7A H 0.5129 1.1116 0.3048 0.291 Uiso 1 1 calc R
H7B H 0.4100 1.0294 0.1686 0.291 Uiso 1 1 calc R
H7C H 0.5041 0.9576 0.2622 0.291 Uiso 1 1 calc R
C8 C 0.1907(6) 0.9261(5) 0.4617(5) 0.0648(15) Uani 1 1 d .
H8A H 0.1862 0.8765 0.5186 0.097 Uiso 1 1 calc R
H8B H 0.1022 0.9631 0.4361 0.097 Uiso 1 1 calc R
H8C H 0.2672 0.9955 0.5055 0.097 Uiso 1 1 calc R
C9 C 0.3523(5) 0.7776(5) 0.3857(5) 0.0609(14) Uani 1 1 d .
H9A H 0.3714 0.7757 0.4736 0.073 Uiso 1 1 calc R
H9B H 0.4299 0.8325 0.3848 0.073 Uiso 1 1 calc R
C10 C 0.3486(5) 0.6402(5) 0.3003(5) 0.0556(13) Uani 1 1 d .
H10A H 0.3100 0.6382 0.2108 0.067 Uiso 1 1 calc R
H10B H 0.4450 0.6154 0.3157 0.067 Uiso 1 1 calc R
C11 C 0.2602(5) 0.5440(5) 0.3247(4) 0.0454(11) Uani 1 1 d .
C12 C 0.3175(5) 0.4423(5) 0.3718(5) 0.0564(13) Uani 1 1 d .
H12 H 0.4120 0.4277 0.3812 0.068 Uiso 1 1 calc R
C13 C 0.2358(6) 0.3641(5) 0.4042(5) 0.0616(14) Uani 1 1 d .
H13 H 0.2740 0.2960 0.4354 0.074 Uiso 1 1 calc R
C14 C 0.0947(6) 0.3870(5) 0.3901(5) 0.0523(12) Uani 1 1 d .
H14 H 0.0373 0.3362 0.4135 0.063 Uiso 1 1 calc R
C15 C 0.0428(5) 0.4861(5) 0.3411(4) 0.0481(11) Uani 1 1 d .
H15 H -0.0522 0.5003 0.3297 0.058 Uiso 1 1 calc R
O1 O 0.3194(4) 1.0262(4) 0.3202(4) 0.0737(11) 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'
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
N3 Cu1 N1 173.11(15) . .
N3 Cu1 N4 92.97(15) . .
N1 Cu1 N4 93.50(16) . .
N3 Cu1 N2 91.84(15) . .
N1 Cu1 N2 81.61(16) . .
N4 Cu1 N2 174.81(15) . .
N10 Cu2 N13 98.7(2) . 2_465
N10 Cu2 N9 91.2(2) . .
N13 Cu2 N9 168.98(17) 2_465 .
N10 Cu2 N13 167.6(2) . .
N13 Cu2 N13 76.59(18) 2_465 .
N9 Cu2 N13 92.72(17) . .
C5 N1 C1 119.5(4) . .
C5 N1 Cu1 115.1(3) . .
C1 N1 Cu1 124.7(3) . .
C6 N2 C8 110.4(4) . .
C6 N2 C9 110.1(4) . .
C8 N2 C9 109.2(4) . .
C6 N2 Cu1 102.2(3) . .
C8 N2 Cu1 109.6(3) . .
C9 N2 Cu1 115.1(3) . .
C11 N3 C15 118.5(4) . .
C11 N3 Cu1 121.4(3) . .
C15 N3 Cu1 120.0(3) . .
N5 N4 Cu1 117.9(3) . .
N6 N5 N4 177.1(5) . .
N7 N8 N9 178.4(5) . .
N8 N9 Cu2 112.5(3) . .
N11 N10 Cu2 137.9(5) . .
N12 N11 N10 174.2(7) . .
N14 N13 Cu2 129.2(4) . 2_465
N14 N13 Cu2 127.2(4) . .
Cu2 N13 Cu2 103.41(18) 2_465 .
N15 N14 N13 178.4(7) . .
N1 C1 C2 121.4(5) . .
C1 C2 C3 118.4(6) . .
C4 C3 C2 120.1(5) . .
C5 C4 C3 118.6(6) . .
N1 C5 C4 122.0(5) . .
N1 C5 C6 113.3(4) . .
C4 C5 C6 124.7(5) . .
O1 C6 N2 111.0(4) . .
O1 C6 C5 110.5(4) . .
N2 C6 C5 107.7(4) . .
N2 C9 C10 112.9(4) . .
C11 C10 C9 111.5(4) . .
N3 C11 C12 120.3(5) . .
N3 C11 C10 117.1(4) . .
C12 C11 C10 122.4(4) . .
C13 C12 C11 120.4(5) . .
C12 C13 C14 119.3(5) . .
C15 C14 C13 118.1(5) . .
N3 C15 C14 123.3(5) . .
C6 O1 C7 112.9(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N3 1.973(4) .
Cu1 N1 1.978(4) .
Cu1 N4 2.018(4) .
Cu1 N2 2.097(4) .
Cu2 N10 1.915(5) .
Cu2 N13 1.972(4) 2_465
Cu2 N9 1.983(4) .
Cu2 N13 2.005(4) .
N1 C5 1.334(6) .
N1 C1 1.344(6) .
N2 C6 1.489(6) .
N2 C8 1.496(6) .
N2 C9 1.497(6) .
N3 C11 1.349(6) .
N3 C15 1.351(6) .
N4 N5 1.194(5) .
N5 N6 1.152(5) .
N7 N8 1.158(5) .
N8 N9 1.200(5) .
N10 N11 1.137(6) .
N11 N12 1.105(7) .
N13 N14 1.179(5) .
N13 Cu2 1.972(4) 2_465
N14 N15 1.116(6) .
C1 C2 1.376(7) .
C2 C3 1.378(9) .
C3 C4 1.372(9) .
C4 C5 1.369(7) .
C5 C6 1.522(7) .
C6 O1 1.400(6) .
C7 O1 1.685(12) .
C9 C10 1.504(7) .
C10 C11 1.486(7) .
C11 C12 1.393(6) .
C12 C13 1.360(7) .
C13 C14 1.390(7) .
C14 C15 1.364(6) .
