#------------------------------------------------------------------------------
#$Date: 2016-03-25 14:07:06 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179880 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/76/7017665.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_7017665
loop_
_publ_author_name
'Mukherjee, Sandip'
'Patil, Yogesh P.'
'Mukherjee, Partha Sarathi'
_publ_section_title
;
 Cu(II)-azide polymers with various molar equivalents of blocking diamine
 ligands: synthesis, structures, magnetic properties with DFT studies.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              54
_journal_page_last               64
_journal_paper_doi               10.1039/c1dt11312g
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         'C8 H24 Cu5 N34'
_chemical_formula_sum            'C8 H24 Cu5 N34'
_chemical_formula_weight         914.31
_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                113.678(2)
_cell_angle_beta                 92.067(2)
_cell_angle_gamma                93.776(2)
_cell_formula_units_Z            1
_cell_length_a                   7.6737(3)
_cell_length_b                   9.4801(4)
_cell_length_c                   11.3796(5)
_cell_measurement_reflns_used    4513
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.5
_cell_measurement_theta_min      2.3
_cell_volume                     754.73(6)
_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 0.983
_diffrn_measured_fraction_theta_max 0.983
_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  0.0246
_diffrn_reflns_av_sigmaI/netI    0.0320
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11543
_diffrn_reflns_theta_full        30.50
_diffrn_reflns_theta_max         30.50
_diffrn_reflns_theta_min         2.35
_exptl_absorpt_coefficient_mu    3.534
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5790
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.012
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             455
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.645
_refine_diff_density_min         -0.389
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         4513
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0279
_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)+(0.0370P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0677
_refine_ls_wR_factor_ref         0.0714
_reflns_number_gt                3660
_reflns_number_total             4513
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c1dt11312g.txt
_cod_data_source_block           complex3
_cod_original_cell_volume        754.73(5)
_cod_database_code               7017665
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 0.18929(3) 0.36741(3) 0.32068(2) 0.02734(7) Uani 1 1 d .
Cu2 Cu 0.14263(3) 0.09736(3) 0.44589(2) 0.02466(7) Uani 1 1 d .
Cu3 Cu 0.5000 0.0000 0.5000 0.02559(8) Uani 1 2 d S
N1 N 0.1918(2) 0.3395(2) 0.13285(16) 0.0328(4) Uani 1 1 d .
N2 N 0.4412(2) 0.3248(2) 0.30563(17) 0.0346(4) Uani 1 1 d .
H2A H 0.5072 0.4009 0.3696 0.042 Uiso 1 1 calc R
H2B H 0.4557 0.2352 0.3131 0.042 Uiso 1 1 calc R
N3 N 0.2261(2) 0.4166(2) 0.50974(16) 0.0314(4) Uani 1 1 d .
N4 N 0.13256(19) 0.48673(18) 0.58731(15) 0.0247(3) Uani 1 1 d .
N5 N 0.0476(2) 0.5545(2) 0.67111(17) 0.0347(4) Uani 1 1 d .
N6 N 0.0465(2) 0.1202(2) 0.29388(17) 0.0324(4) Uani 1 1 d .
N7 N -0.1069(2) 0.0910(2) 0.25843(16) 0.0316(4) Uani 1 1 d .
N8 N -0.2513(3) 0.0646(3) 0.2198(2) 0.0538(6) Uani 1 1 d .
N9 N -0.0456(2) 0.1675(2) 0.56393(17) 0.0324(4) Uani 1 1 d .
N10 N -0.1731(2) 0.22855(19) 0.55194(17) 0.0288(3) Uani 1 1 d .
N11 N -0.2989(3) 0.2846(3) 0.5464(2) 0.0511(5) Uani 1 1 d .
N12 N 0.3567(2) 0.0079(2) 0.35385(15) 0.0292(4) Uani 1 1 d .
N13 N 0.3488(2) -0.0756(2) 0.24009(17) 0.0332(4) Uani 1 1 d .
N14 N 0.3392(3) -0.1493(3) 0.1335(2) 0.0651(7) Uani 1 1 d .
N15 N 0.3121(2) 0.1192(2) 0.59305(16) 0.0294(4) Uani 1 1 d .
N16 N 0.3108(2) 0.2225(2) 0.69711(18) 0.0345(4) Uani 1 1 d .
N17 N 0.3048(4) 0.3213(3) 0.7950(2) 0.0692(7) Uani 1 1 d .
C1 C 0.3485(3) 0.2546(4) 0.0849(2) 0.0571(7) Uani 1 1 d .
H1A H 0.3210 0.1457 0.0647 0.069 Uiso 1 1 calc R
H1B H 0.3795 0.2645 0.0065 0.069 Uiso 1 1 calc R
C2 C 0.4984(3) 0.3150(4) 0.1811(2) 0.0524(7) Uani 1 1 d .
H2C H 0.5918 0.2469 0.1549 0.063 Uiso 1 1 calc R
H2D H 0.5426 0.4165 0.1883 0.063 Uiso 1 1 calc R
C3 C 0.2071(4) 0.4926(3) 0.1283(3) 0.0579(7) Uani 1 1 d .
H3A H 0.3076 0.5532 0.1818 0.087 Uiso 1 1 calc R
H3B H 0.1037 0.5438 0.1588 0.087 Uiso 1 1 calc R
H3C H 0.2200 0.4808 0.0413 0.087 Uiso 1 1 calc R
C4 C 0.0376(3) 0.2482(4) 0.0513(2) 0.0581(7) Uani 1 1 d .
H4A H 0.0269 0.1479 0.0537 0.087 Uiso 1 1 calc R
H4B H 0.0502 0.2370 -0.0355 0.087 Uiso 1 1 calc R
H4C H -0.0654 0.2999 0.0825 0.087 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
N5 Cu1 N2 168.93(8) 2_566 .
N5 Cu1 N3 96.30(7) 2_566 .
N2 Cu1 N3 87.58(7) . .
N5 Cu1 N1 89.42(7) 2_566 .
N2 Cu1 N1 85.40(7) . .
N3 Cu1 N1 170.20(7) . .
N5 Cu1 N6 88.06(7) 2_566 .
N2 Cu1 N6 102.49(7) . .
N3 Cu1 N6 87.78(6) . .
N1 Cu1 N6 100.40(7) . .
N6 Cu2 N9 101.56(7) . .
N6 Cu2 N15 159.79(7) . .
N9 Cu2 N15 90.89(7) . .
N6 Cu2 N12 91.03(7) . .
N9 Cu2 N12 167.11(7) . .
N15 Cu2 N12 77.81(6) . .
N15 Cu3 N15 180.00(10) 2_656 .
N15 Cu3 N12 80.00(6) 2_656 2_656
N15 Cu3 N12 100.00(6) . 2_656
N15 Cu3 N12 100.00(6) 2_656 .
N15 Cu3 N12 80.00(6) . .
N12 Cu3 N12 180.0 2_656 .
C4 N1 C3 109.0(2) . .
C4 N1 C1 108.3(2) . .
C3 N1 C1 111.5(2) . .
C4 N1 Cu1 114.35(14) . .
C3 N1 Cu1 108.98(14) . .
C1 N1 Cu1 104.63(14) . .
C2 N2 Cu1 110.28(13) . .
C2 N2 H2A 109.6 . .
Cu1 N2 H2A 109.6 . .
C2 N2 H2B 109.6 . .
Cu1 N2 H2B 109.6 . .
H2A N2 H2B 108.1 . .
N4 N3 Cu1 124.09(14) . .
N5 N4 N3 174.87(19) . .
N4 N5 Cu1 133.97(15) . 2_566
N7 N6 Cu2 122.53(14) . .
N7 N6 Cu1 119.03(14) . .
Cu2 N6 Cu1 101.58(7) . .
N8 N7 N6 176.8(2) . .
N10 N9 Cu2 128.67(15) . .
N11 N10 N9 175.7(2) . .
N13 N12 Cu3 130.20(14) . .
N13 N12 Cu2 122.23(13) . .
Cu3 N12 Cu2 99.64(7) . .
N14 N13 N12 177.7(2) . .
N16 N15 Cu3 132.20(14) . .
N16 N15 Cu2 121.99(13) . .
Cu3 N15 Cu2 101.02(7) . .
N17 N16 N15 178.0(2) . .
C2 C1 N1 111.3(2) . .
C2 C1 H1A 109.4 . .
N1 C1 H1A 109.4 . .
C2 C1 H1B 109.4 . .
N1 C1 H1B 109.4 . .
H1A C1 H1B 108.0 . .
N2 C2 C1 108.95(19) . .
N2 C2 H2C 109.9 . .
C1 C2 H2C 109.9 . .
N2 C2 H2D 109.9 . .
C1 C2 H2D 109.9 . .
H2C C2 H2D 108.3 . .
N1 C3 H3A 109.5 . .
N1 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
N1 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
N1 C4 H4A 109.5 . .
N1 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
N1 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N5 1.9991(17) 2_566
Cu1 N2 2.0005(16) .
Cu1 N3 2.0147(17) .
Cu1 N1 2.0465(17) .
Cu1 N6 2.4185(18) .
Cu2 N6 1.9527(16) .
Cu2 N9 1.9700(16) .
Cu2 N15 2.0165(16) .
Cu2 N12 2.0268(15) .
Cu3 N15 1.9602(15) 2_656
Cu3 N15 1.9602(15) .
Cu3 N12 1.9901(16) 2_656
Cu3 N12 1.9901(16) .
N1 C4 1.467(3) .
N1 C3 1.470(3) .
N1 C1 1.488(3) .
N2 C2 1.467(3) .
N2 H2A 0.9000 .
N2 H2B 0.9000 .
N3 N4 1.172(2) .
N4 N5 1.164(2) .
N5 Cu1 1.9991(17) 2_566
N6 N7 1.208(2) .
N7 N8 1.150(2) .
N9 N10 1.200(2) .
N10 N11 1.144(2) .
N12 N13 1.213(2) .
N13 N14 1.127(3) .
N15 N16 1.197(2) .
N16 N17 1.136(3) .
C1 C2 1.473(4) .
C1 H1A 0.9700 .
C1 H1B 0.9700 .
C2 H2C 0.9700 .
C2 H2D 0.9700 .
C3 H3A 0.9600 .
C3 H3B 0.9600 .
C3 H3C 0.9600 .
C4 H4A 0.9600 .
C4 H4B 0.9600 .
C4 H4C 0.9600 .
