#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:32:24 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179250 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/70/4317081.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_4317081
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         'C4 H12 Cu3 N20'
_chemical_formula_sum            'C4 H12 Cu3 N20'
_chemical_formula_weight         530.96
_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                99.827(2)
_cell_angle_beta                 102.911(2)
_cell_angle_gamma                113.017(2)
_cell_formula_units_Z            2
_cell_length_a                   8.4648(3)
_cell_length_b                   10.5388(5)
_cell_length_c                   11.3126(6)
_cell_measurement_temperature    296(2)
_cell_volume                     867.10(7)
_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      296(2)
_diffrn_measured_fraction_theta_full 0.951
_diffrn_measured_fraction_theta_max 0.951
_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  0.0301
_diffrn_reflns_av_sigmaI/netI    0.0559
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_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            9896
_diffrn_reflns_theta_full        30.47
_diffrn_reflns_theta_max         30.47
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    3.687
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.4923
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.034
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             526
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.660
_refine_diff_density_min         -0.620
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         4997
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0380
_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)+(0.0398P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0832
_refine_ls_wR_factor_ref         0.0936
_reflns_number_gt                3567
_reflns_number_total             4997
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ic1016966_si_002_3.cif
_cod_data_source_block           complex3
_cod_database_code               4317081
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
Cu2 Cu 0.11200(4) 0.40309(4) 0.06985(3) 0.02704(10) Uani 1 1 d . . .
Cu3 Cu 0.26692(4) 0.57630(4) -0.10849(4) 0.02788(10) Uani 1 1 d . . .
Cu1 Cu -0.04643(5) 0.28888(4) 0.28548(4) 0.03018(11) Uani 1 1 d . . .
N12 N 0.3429(3) 0.5649(3) 0.0705(3) 0.0347(6) Uani 1 1 d . . .
N3 N -0.1343(3) 0.2628(3) 0.0600(2) 0.0296(5) Uani 1 1 d . . .
N16 N 0.1282(3) 0.4787(3) -0.3842(3) 0.0319(6) Uani 1 1 d . . .
N13 N 0.4943(3) 0.6010(2) 0.1377(2) 0.0290(5) Uani 1 1 d . . .
N9 N 0.0445(3) 0.4117(2) -0.1080(2) 0.0297(5) Uani 1 1 d . . .
N2 N -0.2859(3) 0.1356(3) 0.2813(3) 0.0374(6) Uani 1 1 d . . .
H2 H -0.3722 0.1377 0.2181 0.045 Uiso 1 1 calc R . .
N19 N 0.6446(4) 0.7578(3) -0.0614(3) 0.0339(6) Uani 1 1 d . . .
N6 N 0.1762(3) 0.4231(3) 0.2540(3) 0.0358(6) Uani 1 1 d . . .
N18 N 0.4918(4) 0.7329(3) -0.1017(3) 0.0520(9) Uani 1 1 d . . .
N15 N 0.1470(3) 0.5641(3) -0.2902(2) 0.0343(6) Uani 1 1 d . . .
N4 N -0.2233(3) 0.1546(3) -0.0274(3) 0.0384(7) Uani 1 1 d . . .
N10 N -0.0552(4) 0.3112(3) -0.2018(3) 0.0413(7) Uani 1 1 d . . .
N1 N 0.0338(4) 0.1309(3) 0.2742(3) 0.0429(7) Uani 1 1 d . . .
H1 H 0.0311 0.1034 0.1927 0.052 Uiso 1 1 calc R . .
N7 N 0.3045(4) 0.5225(3) 0.3333(3) 0.0518(8) Uani 1 1 d . . .
N17 N 0.1090(5) 0.3986(3) -0.4735(3) 0.0563(9) Uani 1 1 d . . .
N14 N 0.6376(4) 0.6358(3) 0.2027(3) 0.0516(8) Uani 1 1 d . . .
N20 N 0.7986(4) 0.7917(3) -0.0218(4) 0.0599(10) Uani 1 1 d . . .
N11 N -0.1470(6) 0.2200(4) -0.2896(4) 0.0924(15) Uani 1 1 d . . .
N5 N -0.3085(5) 0.0513(3) -0.1069(4) 0.0792(12) Uani 1 1 d . . .
C2 C -0.2844(5) -0.0049(4) 0.2383(5) 0.0748(15) Uani 1 1 d . . .
H2A H -0.3726 -0.0775 0.2630 0.090 Uiso 1 1 calc R . .
H2B H -0.3176 -0.0344 0.1467 0.090 Uiso 1 1 calc R . .
N8 N 0.4267(5) 0.6149(5) 0.4080(4) 0.119(2) Uani 1 1 d . . .
C3 C 0.2133(5) 0.1653(4) 0.3534(5) 0.0674(13) Uani 1 1 d . . .
H3A H 0.3013 0.2461 0.3381 0.101 Uiso 1 1 calc R . .
H3B H 0.2376 0.0838 0.3340 0.101 Uiso 1 1 calc R . .
H3C H 0.2202 0.1888 0.4408 0.101 Uiso 1 1 calc R . .
C1 C -0.1071(5) 0.0065(4) 0.2933(5) 0.0757(15) Uani 1 1 d . . .
H1A H -0.1023 -0.0810 0.2549 0.091 Uiso 1 1 calc R . .
H1B H -0.0839 0.0172 0.3833 0.091 Uiso 1 1 calc R . .
C4 C -0.3381(5) 0.1555(5) 0.3946(4) 0.0677(12) Uani 1 1 d . . .
H4A H -0.3337 0.2492 0.4166 0.101 Uiso 1 1 calc R . .
H4B H -0.2561 0.1471 0.4631 0.101 Uiso 1 1 calc R . .
H4C H -0.4590 0.0833 0.3788 0.101 Uiso 1 1 calc R . .
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
_geom_angle_publ_flag
N6 Cu2 N9 171.01(10) . . ?
N6 Cu2 N3 85.32(10) . . ?
N9 Cu2 N3 96.23(10) . . ?
N6 Cu2 N12 98.65(10) . . ?
N9 Cu2 N12 78.58(10) . . ?
N3 Cu2 N12 170.81(10) . . ?
N6 Cu2 N20 93.72(12) . 2_665 ?
N9 Cu2 N20 95.09(12) . 2_665 ?
N3 Cu2 N20 91.50(10) . 2_665 ?
N12 Cu2 N20 96.48(11) . 2_665 ?
N18 Cu3 N9 176.53(11) . . ?
N18 Cu3 N12 98.53(12) . . ?
N9 Cu3 N12 78.49(10) . . ?
N18 Cu3 N15 91.17(12) . . ?
N9 Cu3 N15 91.86(10) . . ?
N12 Cu3 N15 170.16(10) . . ?
N18 Cu3 N3 92.73(11) . 2_565 ?
N9 Cu3 N3 89.34(9) . 2_565 ?
N12 Cu3 N3 95.14(10) . 2_565 ?
N15 Cu3 N3 82.73(9) . 2_565 ?
N6 Cu1 N2 169.08(11) . . ?
N6 Cu1 N1 91.98(11) . . ?
N2 Cu1 N1 85.41(11) . . ?
N6 Cu1 N15 91.54(11) . 2_565 ?
N2 Cu1 N15 90.65(11) . 2_565 ?
N1 Cu1 N15 175.62(10) . 2_565 ?
N6 Cu1 N3 74.03(9) . . ?
N2 Cu1 N3 95.65(10) . . ?
N1 Cu1 N3 95.82(11) . . ?
N15 Cu1 N3 82.66(9) 2_565 . ?
N13 N12 Cu3 127.4(2) . . ?
N13 N12 Cu2 126.6(2) . . ?
Cu3 N12 Cu2 100.47(11) . . ?
N4 N3 Cu2 121.4(2) . . ?
N4 N3 Cu3 118.5(2) . 2_565 ?
Cu2 N3 Cu3 100.78(10) . 2_565 ?
N4 N3 Cu1 129.1(2) . . ?
Cu2 N3 Cu1 93.17(9) . . ?
Cu3 N3 Cu1 85.68(8) 2_565 . ?
N17 N16 N15 179.3(4) . . ?
N14 N13 N12 179.3(4) . . ?
N10 N9 Cu2 126.8(2) . . ?
N10 N9 Cu3 122.5(2) . . ?
Cu2 N9 Cu3 102.37(11) . . ?
C4 N2 C2 114.8(3) . . ?
C4 N2 Cu1 116.6(2) . . ?
C2 N2 Cu1 106.6(2) . . ?
N20 N19 N18 175.5(3) . . ?
N7 N6 Cu2 124.5(2) . . ?
N7 N6 Cu1 125.2(2) . . ?
Cu2 N6 Cu1 107.46(11) . . ?
N19 N18 Cu3 132.8(2) . . ?
N16 N15 Cu3 126.1(2) . . ?
N16 N15 Cu1 125.6(2) . 2_565 ?
Cu3 N15 Cu1 108.16(12) . 2_565 ?
N5 N4 N3 178.0(4) . . ?
N11 N10 N9 178.8(4) . . ?
C3 N1 C1 111.8(3) . . ?
C3 N1 Cu1 118.0(2) . . ?
C1 N1 Cu1 107.2(2) . . ?
N8 N7 N6 178.9(5) . . ?
N19 N20 Cu2 115.2(2) . 2_665 ?
C1 C2 N2 110.1(3) . . ?
C2 C1 N1 110.9(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
Cu2 N6 1.983(3) . ?
Cu2 N9 1.993(3) . ?
Cu2 N3 1.994(2) . ?
Cu2 N12 2.028(2) . ?
Cu2 N20 2.470(3) 2_665 ?
Cu3 N18 1.946(3) . ?
Cu3 N9 2.002(2) . ?
Cu3 N12 2.022(3) . ?
Cu3 N15 2.036(3) . ?
Cu3 N3 2.425(3) 2_565 ?
Cu1 N6 2.016(2) . ?
Cu1 N2 2.022(2) . ?
Cu1 N1 2.024(3) . ?
Cu1 N15 2.038(2) 2_565 ?
Cu1 N3 2.427(3) . ?
N12 N13 1.204(3) . ?
N3 N4 1.207(3) . ?
N3 Cu3 2.425(2) 2_565 ?
N16 N17 1.135(4) . ?
N16 N15 1.205(4) . ?
N13 N14 1.144(3) . ?
N9 N10 1.215(3) . ?
N2 C4 1.454(5) . ?
N2 C2 1.485(4) . ?
N19 N20 1.161(4) . ?
N19 N18 1.175(3) . ?
N6 N7 1.198(4) . ?
N15 Cu1 2.038(2) 2_565 ?
N4 N5 1.129(4) . ?
N10 N11 1.122(4) . ?
N1 C3 1.447(4) . ?
N1 C1 1.476(4) . ?
N7 N8 1.129(4) . ?
N20 Cu2 2.470(3) 2_665 ?
C2 C1 1.439(5) . ?
