#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:32:24 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179250 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/70/4317080.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_4317080
loop_
_publ_author_name
'Sandip Mukherjee'
'Partha Sarathi Mukherjee'
_publ_section_title
;
 A Series of CuII-Azide Polymers of Cu6 Building Units and the Role of
 Chelating Diamine in Controlling their Dimensionality: Synthesis,
 Structures, and Magnetic Behavior
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10658
_journal_page_last               10667
_journal_paper_doi               10.1021/ic1016966
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C6 H16 Cu3 N20 O'
_chemical_formula_sum            'C6 H16 Cu3 N20 O'
_chemical_formula_weight         575.01
_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                94.050(3)
_cell_angle_beta                 100.111(3)
_cell_angle_gamma                111.710(3)
_cell_formula_units_Z            2
_cell_length_a                   9.6797(5)
_cell_length_b                   10.2117(5)
_cell_length_c                   11.0171(5)
_cell_measurement_temperature    293(2)
_cell_volume                     985.04(9)
_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 0.935
_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  0.0658
_diffrn_reflns_av_sigmaI/netI    0.0852
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            19930
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.53
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    3.257
_exptl_absorpt_correction_T_max  0.536
_exptl_absorpt_correction_T_min  0.439
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.939
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             574
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.096
_refine_diff_density_min         -0.605
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         5634
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.1066
_refine_ls_R_factor_gt           0.0493
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0569P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1085
_refine_ls_wR_factor_ref         0.1301
_reflns_number_gt                3331
_reflns_number_total             5634
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ic1016966_si_002_2.cif
_cod_data_source_block           complex2
_cod_original_cell_volume        985.04(8)
_cod_database_code               4317080
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
Cu3 Cu 0.01847(6) 0.25663(5) 0.44296(5) 0.03058(15) Uani 1 1 d . . .
Cu2 Cu -0.11500(6) 0.02539(5) 0.60821(4) 0.02947(15) Uani 1 1 d . . .
Cu1 Cu -0.18139(6) -0.21744(5) 0.79578(5) 0.02931(15) Uani 1 1 d . . .
N7 N -0.0309(4) 0.0848(4) 0.8824(3) 0.0291(8) Uani 1 1 d . . .
N3 N -0.2393(4) -0.1816(4) 0.5796(3) 0.0315(8) Uani 1 1 d . . .
N9 N -0.1196(4) 0.0499(4) 0.4294(3) 0.0346(9) Uani 1 1 d . . .
N12 N 0.0225(5) 0.2293(4) 0.6234(3) 0.0389(9) Uani 1 1 d . . .
N6 N -0.0855(4) -0.0022(4) 0.7891(3) 0.0338(9) Uani 1 1 d . . .
N10 N -0.2251(5) -0.0185(4) 0.3434(4) 0.0416(10) Uani 1 1 d . . .
N15 N 0.0016(4) 0.2398(4) 0.2567(3) 0.0341(9) Uani 1 1 d . . .
N13 N 0.1017(5) 0.3134(4) 0.7131(4) 0.0440(10) Uani 1 1 d . . .
N16 N -0.1126(5) 0.2320(4) 0.1861(3) 0.0399(10) Uani 1 1 d . . .
N4 N -0.3574(4) -0.2468(4) 0.5061(3) 0.0373(9) Uani 1 1 d . . .
N8 N 0.0181(5) 0.1644(4) 0.9721(3) 0.0470(11) Uani 1 1 d . . .
N11 N -0.3221(7) -0.0838(6) 0.2628(5) 0.093(2) Uani 1 1 d . . .
N17 N -0.2188(6) 0.2248(7) 0.1184(4) 0.0784(17) Uani 1 1 d . . .
N5 N -0.4702(5) -0.3138(6) 0.4396(5) 0.0742(16) Uani 1 1 d . . .
N19 N 0.1829(4) 0.5556(4) 0.5228(3) 0.0323(8) Uani 1 1 d . . .
N18 N 0.1815(5) 0.4501(4) 0.4747(4) 0.0499(11) Uani 1 1 d . . .
N14 N 0.1757(7) 0.3938(6) 0.7994(5) 0.099(2) Uani 1 1 d . . .
N1 N -0.3745(4) -0.2099(4) 0.8430(3) 0.0365(9) Uani 1 1 d . . .
N2 N -0.2825(4) -0.4307(4) 0.7919(3) 0.0356(9) Uani 1 1 d . . .
H2 H -0.3051 -0.4705 0.7107 0.043 Uiso 1 1 calc R . .
N20 N 0.1937(5) 0.6652(4) 0.5705(5) 0.0569(12) Uani 1 1 d . . .
C5 C -0.1898(7) -0.5012(5) 0.8633(5) 0.0576(15) Uani 1 1 d . . .
H5A H -0.0874 -0.4617 0.8487 0.069 Uiso 1 1 calc R . .
H5B H -0.1828 -0.4772 0.9516 0.069 Uiso 1 1 calc R . .
C3 C -0.4364(7) -0.1174(8) 0.7747(6) 0.078(2) Uani 1 1 d . . .
H3A H -0.4518 -0.1448 0.6867 0.117 Uiso 1 1 calc R . .
H3B H -0.3659 -0.0199 0.7980 0.117 Uiso 1 1 calc R . .
H3C H -0.5319 -0.1272 0.7951 0.117 Uiso 1 1 calc R . .
C2 C -0.4269(6) -0.4642(6) 0.8290(6) 0.0638(17) Uani 1 1 d . . .
H2A H -0.4989 -0.5567 0.7851 0.077 Uiso 1 1 calc R . .
H2B H -0.4127 -0.4689 0.9177 0.077 Uiso 1 1 calc R . .
C4 C -0.3536(7) -0.1656(8) 0.9753(5) 0.091(3) Uani 1 1 d . . .
H4A H -0.3131 -0.2241 1.0221 0.136 Uiso 1 1 calc R . .
H4B H -0.4500 -0.1756 0.9940 0.136 Uiso 1 1 calc R . .
H4C H -0.2841 -0.0677 0.9975 0.136 Uiso 1 1 calc R . .
C1 C -0.4872(7) -0.3580(6) 0.8012(8) 0.088(2) Uani 1 1 d . . .
H1A H -0.5726 -0.3726 0.8409 0.106 Uiso 1 1 calc R . .
H1B H -0.5253 -0.3705 0.7119 0.106 Uiso 1 1 calc R . .
C6 C -0.2489(8) -0.6574(6) 0.8324(6) 0.078(2) Uani 1 1 d . . .
H6A H -0.1823 -0.6928 0.8820 0.117 Uiso 1 1 calc R . .
H6B H -0.2541 -0.6828 0.7456 0.117 Uiso 1 1 calc R . .
H6C H -0.3489 -0.6985 0.8493 0.117 Uiso 1 1 calc R . .
O1W O -0.3499(6) 0.0940(5) 0.5638(4) 0.0885(15) 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
_geom_angle_publ_flag
N18 Cu3 N9 169.79(17) . . ?
N18 Cu3 N15 93.25(16) . . ?
N9 Cu3 N15 91.66(15) . . ?
N18 Cu3 N12 96.92(16) . . ?
N9 Cu3 N12 77.36(14) . . ?
N15 Cu3 N12 168.15(15) . . ?
N18 Cu3 N20 96.05(16) . 2_566 ?
N9 Cu3 N20 92.67(15) . 2_566 ?
N15 Cu3 N20 92.42(15) . 2_566 ?
N12 Cu3 N20 92.52(16) . 2_566 ?
N3 Cu2 N12 173.66(15) . . ?
N3 Cu2 N9 97.06(14) . . ?
N12 Cu2 N9 78.49(14) . . ?
N3 Cu2 N6 83.53(14) . . ?
N12 Cu2 N6 100.32(14) . . ?
N9 Cu2 N6 172.83(15) . . ?
N15 Cu1 N2 90.52(15) 2_556 . ?
N15 Cu1 N1 175.73(15) 2_556 . ?
N2 Cu1 N1 85.63(15) . . ?
N15 Cu1 N6 89.66(15) 2_556 . ?
N2 Cu1 N6 176.64(14) . . ?
N1 Cu1 N6 94.08(15) . . ?
N15 Cu1 N3 81.99(13) 2_556 . ?
N2 Cu1 N3 104.63(13) . . ?
N1 Cu1 N3 97.19(14) . . ?
N6 Cu1 N3 72.07(12) . . ?
N8 N7 N6 178.1(4) . . ?
N4 N3 Cu2 128.5(3) . . ?
N4 N3 Cu1 125.4(3) . . ?
Cu2 N3 Cu1 96.02(13) . . ?
N10 N9 Cu2 124.7(3) . . ?
N10 N9 Cu3 126.2(3) . . ?
Cu2 N9 Cu3 102.04(15) . . ?
N13 N12 Cu2 130.7(3) . . ?
N13 N12 Cu3 126.8(3) . . ?
Cu2 N12 Cu3 102.11(15) . . ?
N7 N6 Cu2 130.1(3) . . ?
N7 N6 Cu1 122.0(3) . . ?
Cu2 N6 Cu1 107.79(15) . . ?
N11 N10 N9 178.7(6) . . ?
N16 N15 Cu1 124.9(3) . 2_556 ?
N16 N15 Cu3 121.5(3) . . ?
Cu1 N15 Cu3 113.32(18) 2_556 . ?
N14 N13 N12 179.0(6) . . ?
N17 N16 N15 179.0(5) . . ?
N5 N4 N3 176.8(5) . . ?
N18 N19 N20 175.7(5) . . ?
N19 N18 Cu3 129.1(3) . . ?
C4 N1 C3 107.7(5) . . ?
C4 N1 C1 112.2(5) . . ?
C3 N1 C1 106.6(5) . . ?
C4 N1 Cu1 112.9(3) . . ?
C3 N1 Cu1 114.4(3) . . ?
C1 N1 Cu1 102.8(3) . . ?
C2 N2 C5 110.9(4) . . ?
C2 N2 Cu1 109.2(3) . . ?
C5 N2 Cu1 117.0(3) . . ?
N19 N20 Cu3 124.0(4) . 2_566 ?
C6 C5 N2 115.4(5) . . ?
C1 C2 N2 110.7(5) . . ?
C2 C1 N1 113.7(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
Cu3 N18 1.980(4) . ?
Cu3 N9 2.015(3) . ?
Cu3 N15 2.020(3) . ?
Cu3 N12 2.022(3) . ?
Cu3 N20 2.450(4) 2_566 ?
Cu2 N3 1.977(3) . ?
Cu2 N12 1.990(3) . ?
Cu2 N9 1.998(3) . ?
Cu2 N6 2.018(3) . ?
Cu1 N15 2.011(4) 2_556 ?
Cu1 N2 2.025(3) . ?
Cu1 N1 2.052(4) . ?
Cu1 N6 2.058(3) . ?
Cu1 N3 2.435(3) . ?
N7 N8 1.141(5) . ?
N7 N6 1.207(5) . ?
N3 N4 1.200(5) . ?
N9 N10 1.212(5) . ?
N12 N13 1.196(5) . ?
N10 N11 1.129(6) . ?
N15 N16 1.207(5) . ?
N15 Cu1 2.011(4) 2_556 ?
N13 N14 1.143(6) . ?
N16 N17 1.133(6) . ?
N4 N5 1.137(5) . ?
N19 N18 1.161(5) . ?
N19 N20 1.162(5) . ?
N1 C4 1.452(6) . ?
N1 C3 1.477(7) . ?
N1 C1 1.481(6) . ?
N2 C2 1.451(6) . ?
N2 C5 1.500(6) . ?
N20 Cu3 2.450(4) 2_566 ?
C5 C6 1.472(7) . ?
C2 C1 1.436(8) . ?
