#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/60/7006074.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_7006074
loop_
_publ_author_name
'Gu, Zhi-Guo'
'Zuo, Jing-Lin'
'You, Xiao-Zeng'
_publ_section_title
;
 A three-dimensional ferromagnet based on linked copper-azido clusters.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4067
_journal_page_last               4072
_journal_paper_doi               10.1039/b708789f
_journal_year                    2007
_chemical_formula_sum            'C6 H21 Cu4.5 N31 O0.5'
_chemical_formula_weight         821.47
_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                105.264(4)
_cell_angle_beta                 101.508(4)
_cell_angle_gamma                105.822(5)
_cell_formula_units_Z            2
_cell_length_a                   10.557(3)
_cell_length_b                   11.849(3)
_cell_length_c                   12.281(3)
_cell_measurement_reflns_used    2954
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.5
_cell_measurement_theta_min      2.8
_cell_volume                     1363.6(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_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  0.0378
_diffrn_reflns_av_sigmaI/netI    0.0694
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6853
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    3.522
_exptl_absorpt_correction_T_max  0.4853
_exptl_absorpt_correction_T_min  0.4180
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   'SADABS; Bruker(2000)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.001
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             817
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.008
_refine_diff_density_min         -1.387
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         4717
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0721
_refine_ls_R_factor_gt           0.0531
_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)+(0.0663P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1389
_refine_ls_wR_factor_ref         0.1445
_reflns_number_gt                3487
_reflns_number_total             4717
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b708789f.txt
_cod_data_source_block           70112em
_cod_original_cell_volume        1363.7(6)
_cod_original_sg_symbol_H-M      p-1
_cod_original_formula_sum        'C6 H21 Cu4.50 N31 O0.50'
_cod_database_code               7006074
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
Cu1 Cu 0.16056(9) 1.14660(7) 1.04443(7) 0.0352(3) Uani 1 1 d . . .
Cu2 Cu 0.16942(9) 0.87803(7) 0.94806(7) 0.0301(2) Uani 1 1 d . . .
Cu3 Cu 0.21818(9) 0.60861(8) 0.90330(8) 0.0353(3) Uani 1 1 d . C .
Cu4 Cu 0.49707(9) 0.86163(7) 0.95186(7) 0.0317(2) Uani 1 1 d . . .
Cu5 Cu 0.5000 1.0000 0.5000 0.0511(4) Uani 1 2 d SU . .
C1 C 0.0198(8) 0.4423(7) 0.6892(7) 0.051(2) Uani 1 1 d . . .
H1A H -0.0712 0.3814 0.6549 0.062 Uiso 1 1 d R A 3
C2 C 0.1154(9) 0.3765(7) 0.7190(7) 0.058(2) Uani 1 1 d D C .
H2A H 0.1236 0.3239 0.6485 0.069 Uiso 1 1 d R B 4
H2B H 0.0818 0.3255 0.7633 0.069 Uiso 1 1 d R B 4
C3 C 0.130(2) 0.2978(18) 0.6080(12) 0.076(7) Uani 0.445(13) 1 d PDU C 1
H3A H 0.0491 0.2250 0.5701 0.114 Uiso 0.445(13) 1 calc PR C 1
H3B H 0.2091 0.2731 0.6270 0.114 Uiso 0.445(13) 1 calc PR C 1
H3C H 0.1424 0.3450 0.5558 0.114 Uiso 0.445(13) 1 calc PR C 1
C3' C 0.053(2) 0.4971(17) 0.5956(13) 0.080(7) Uani 0.555(13) 1 d P C 2
H3'1 H 0.1461 0.5532 0.6236 0.121 Uiso 0.555(13) 1 calc PR C 2
H3'2 H -0.0082 0.5415 0.5786 0.121 Uiso 0.555(13) 1 calc PR C 2
H3'3 H 0.0407 0.4312 0.5251 0.121 Uiso 0.555(13) 1 calc PR C 2
C4 C 0.4383(10) 0.7399(10) 0.4248(10) 0.0854(15) Uani 1 1 d DU . .
H4 H 0.4575 0.7486 0.5086 0.102 Uiso 1 1 d R . .
C5 C 0.5852(10) 0.7897(11) 0.4521(12) 0.110(4) Uani 1 1 d D . .
H5A H 0.5942 0.7520 0.3750 0.132 Uiso 1 1 d R . .
H5B H 0.6353 0.7603 0.5072 0.132 Uiso 1 1 d R . .
C6 C 0.3645(12) 0.6031(9) 0.3972(13) 0.120(5) Uani 1 1 d . . .
H6A H 0.3045 0.5789 0.3190 0.179 Uiso 1 1 d R . .
H6B H 0.3107 0.5880 0.4497 0.179 Uiso 1 1 d R . .
H6C H 0.4248 0.5553 0.3968 0.179 Uiso 1 1 d R . .
N1 N 0.1810(8) 1.2747(6) 0.9713(6) 0.059(2) Uani 1 1 d . . .
N2 N 0.1812(6) 1.3775(6) 1.0056(6) 0.0440(16) Uani 1 1 d . . .
N3 N 0.1806(7) 1.4796(6) 1.0317(6) 0.0534(18) Uani 1 1 d . . .
N4 N 0.1274(6) 0.9866(5) 1.0817(5) 0.0327(14) Uani 1 1 d . . .
N5 N 0.1255(6) 0.9837(6) 1.1774(6) 0.0387(15) Uani 1 1 d . . .
N6 N 0.1193(9) 0.9811(8) 1.2678(7) 0.079(3) Uani 1 1 d . . .
N7 N 0.2013(7) 1.0360(5) 0.9119(5) 0.0412(16) Uani 1 1 d . . .
N8 N 0.2252(6) 1.0595(6) 0.8264(5) 0.0406(15) Uani 1 1 d . . .
N9 N 0.2525(10) 1.0863(7) 0.7512(7) 0.079(3) Uani 1 1 d . . .
N10 N 0.1681(6) 0.7392(5) 1.0101(5) 0.0357(14) Uani 1 1 d . . .
N11 N 0.1635(6) 0.7355(5) 1.1042(6) 0.0366(14) Uani 1 1 d . . .
N12 N 0.1571(8) 0.7278(6) 1.1940(6) 0.063(2) Uani 1 1 d . . .
N13 N 0.2460(6) 0.7925(5) 0.8280(5) 0.0361(14) Uani 1 1 d . . .
N14 N 0.2301(6) 0.7937(6) 0.7294(6) 0.0412(15) Uani 1 1 d . . .
N15 N 0.2185(10) 0.7924(9) 0.6377(7) 0.090(3) Uani 1 1 d . . .
N16 N 0.4194(6) 0.7062(5) 0.9856(5) 0.0375(14) Uani 1 1 d . . .
N17 N 0.4827(6) 0.6694(6) 1.0528(6) 0.0473(16) Uani 1 1 d . . .
N18 N 0.5362(9) 0.6366(9) 1.1202(9) 0.100(3) Uani 1 1 d . . .
N19 N 0.0220(6) 0.5292(5) 0.8020(5) 0.0392(15) Uani 1 1 d . C .
H19A H -0.0300 0.4875 0.8383 0.047 Uiso 1 1 calc R . .
H19B H -0.0118 0.5878 0.7883 0.047 Uiso 1 1 calc R . .
N20 N 0.2526(7) 0.4717(5) 0.7894(5) 0.0483(17) Uani 1 1 d . . .
H20A H 0.2966 0.5018 0.7420 0.058 Uiso 1 1 calc R C .
H20B H 0.3047 0.4381 0.8288 0.058 Uiso 1 1 calc R . .
N21 N 0.5355(6) 1.0218(5) 0.9137(5) 0.0372(14) Uani 1 1 d . . .
N22 N 0.5475(6) 1.0283(5) 0.8203(5) 0.0339(13) Uani 1 1 d . . .
N23 N 0.5613(8) 1.0327(7) 0.7333(6) 0.060(2) Uani 1 1 d . . .
N24 N 0.5872(7) 0.7922(6) 0.8394(6) 0.0460(16) Uani 1 1 d . . .
N25 N 0.5252(8) 0.6963(7) 0.7656(7) 0.059(2) Uani 1 1 d . . .
N26 N 0.4669(11) 0.6036(9) 0.6933(9) 0.116(4) Uani 1 1 d . . .
N27 N 0.3673(7) 0.8263(6) 0.4517(6) 0.0567(13) Uani 1 1 d U . .
H27A H 0.3313 0.8167 0.5106 0.068 Uiso 1 1 calc R . .
H27B H 0.2980 0.8117 0.3878 0.068 Uiso 1 1 calc R . .
N28 N 0.6456(7) 0.9224(7) 0.4848(6) 0.0607(19) Uani 1 1 d . . .
H28A H 0.6836 0.9413 0.4296 0.073 Uiso 1 1 calc R . .
H28B H 0.7125 0.9526 0.5539 0.073 Uiso 1 1 calc R . .
O1W O 0.915(4) 0.073(3) 0.509(2) 0.30(2) Uani 0.50 1 d P . .
H1WA H 0.9591 0.0310 0.5340 0.361 Uiso 0.50 1 d PR . .
H1WB H 0.9153 0.0593 0.4375 0.361 Uiso 0.50 1 d PR . .
N31 N 0.0800(7) 1.2237(6) 1.1616(6) 0.0423(16) Uani 1 1 d . . .
N30 N 0.1279(9) 1.2531(7) 1.2599(7) 0.071(2) Uani 1 1 d . . .
N29 N 0.1750(14) 1.2830(12) 1.3595(12) 0.143(5) Uani 1 1 d U . .
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'
O O 0.0106 0.0060 '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
N1 Cu1 N31 95.5(3) . . ?
N1 Cu1 N7 90.7(2) . . ?
N31 Cu1 N7 166.9(3) . . ?
N1 Cu1 N4 166.7(3) . . ?
N31 Cu1 N4 94.9(2) . . ?
N7 Cu1 N4 77.5(2) . . ?
N10 Cu2 N7 169.3(3) . . ?
N10 Cu2 N13 85.2(2) . . ?
N7 Cu2 N13 97.4(2) . . ?
N10 Cu2 N4 97.7(2) . . ?
N7 Cu2 N4 78.0(2) . . ?
N13 Cu2 N4 169.6(2) . . ?
N19 Cu3 N10 90.2(2) . . ?
N19 Cu3 N20 85.4(3) . . ?
N10 Cu3 N20 175.5(3) . . ?
N19 Cu3 N16 169.7(2) . . ?
N10 Cu3 N16 89.9(2) . . ?
N20 Cu3 N16 94.5(3) . . ?
N24 Cu4 N16 96.3(2) . . ?
N24 Cu4 N21 161.2(3) . 2_677 ?
N16 Cu4 N21 97.1(2) . 2_677 ?
N24 Cu4 N21 92.0(2) . . ?
N16 Cu4 N21 167.8(2) . . ?
N21 Cu4 N21 77.1(2) 2_677 . ?
N27 Cu5 N27 180.000(1) 2_676 . ?
N27 Cu5 N28 93.5(3) 2_676 . ?
N27 Cu5 N28 86.5(3) . . ?
N27 Cu5 N28 86.5(3) 2_676 2_676 ?
N27 Cu5 N28 93.5(3) . 2_676 ?
N28 Cu5 N28 180.000(3) . 2_676 ?
C2 C1 N19 107.1(6) . . ?
C2 C1 C3' 110.2(10) . . ?
N19 C1 C3' 117.4(8) . . ?
C2 C1 H1A 107.6 . . ?
N19 C1 H1A 107.6 . . ?
C3' C1 H1A 106.6 . . ?
C1 C2 N20 108.1(6) . . ?
C1 C2 C3 109.7(10) . . ?
N20 C2 C3 108.3(11) . . ?
C1 C2 H2A 110.5 . . ?
N20 C2 H2A 109.4 . . ?
C3 C2 H2A 1.8 . . ?
C1 C2 H2B 110.1 . . ?
N20 C2 H2B 110.4 . . ?
C3 C2 H2B 110.1 . . ?
H2A C2 H2B 108.3 . . ?
C2 C3 H2A 3.2 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
C1 C3' H3'1 109.5 . . ?
C1 C3' H3'2 109.5 . . ?
H3'1 C3' H3'2 109.5 . . ?
C1 C3' H3'3 109.5 . . ?
H3'1 C3' H3'3 109.5 . . ?
H3'2 C3' H3'3 109.5 . . ?
C5 C4 N27 117.6(9) . . ?
C5 C4 C6 121.1(10) . . ?
N27 C4 C6 119.7(9) . . ?
C5 C4 H4 84.2 . . ?
N27 C4 H4 85.4 . . ?
C6 C4 H4 87.7 . . ?
C4 C5 N28 116.5(9) . . ?
C4 C5 H5A 98.8 . . ?
N28 C5 H5A 108.1 . . ?
C4 C5 H5B 114.9 . . ?
N28 C5 H5B 110.0 . . ?
H5A C5 H5B 107.5 . . ?
C4 C6 H6A 102.5 . . ?
C4 C6 H6B 112.2 . . ?
H6A C6 H6B 109.5 . . ?
C4 C6 H6C 113.4 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N2 N1 Cu1 130.9(5) . . ?
N3 N2 N1 175.2(8) . . ?
N5 N4 Cu2 132.8(4) . . ?
N5 N4 Cu1 122.0(5) . . ?
Cu2 N4 Cu1 101.7(2) . . ?
N6 N5 N4 177.6(8) . . ?
N8 N7 Cu2 130.3(5) . . ?
N8 N7 Cu1 126.4(5) . . ?
Cu2 N7 Cu1 102.9(3) . . ?
N9 N8 N7 176.6(9) . . ?
N11 N10 Cu2 128.4(5) . . ?
N11 N10 Cu3 119.5(4) . . ?
Cu2 N10 Cu3 111.0(3) . . ?
N12 N11 N10 177.8(8) . . ?
N14 N13 Cu2 126.4(5) . . ?
N15 N14 N13 177.5(8) . . ?
N17 N16 Cu4 124.8(5) . . ?
N17 N16 Cu3 118.9(5) . . ?
Cu4 N16 Cu3 116.3(3) . . ?
N18 N17 N16 175.3(9) . . ?
C1 N19 Cu3 107.5(5) . . ?
C1 N19 H19A 110.2 . . ?
Cu3 N19 H19A 110.2 . . ?
C1 N19 H19B 110.2 . . ?
Cu3 N19 H19B 110.2 . . ?
H19A N19 H19B 108.5 . . ?
C2 N20 Cu3 106.7(5) . . ?
C2 N20 H20A 110.4 . . ?
Cu3 N20 H20A 110.4 . . ?
C2 N20 H20B 110.4 . . ?
Cu3 N20 H20B 110.4 . . ?
H20A N20 H20B 108.6 . . ?
N22 N21 Cu4 131.9(5) . 2_677 ?
N22 N21 Cu4 123.7(5) . . ?
Cu4 N21 Cu4 102.9(2) 2_677 . ?
N23 N22 N21 178.0(7) . . ?
N25 N24 Cu4 118.6(6) . . ?
N26 N25 N24 178.8(9) . . ?
C4 N27 Cu5 109.1(6) . . ?
C4 N27 H27A 109.9 . . ?
Cu5 N27 H27A 109.9 . . ?
C4 N27 H27B 109.9 . . ?
Cu5 N27 H27B 109.9 . . ?
H27A N27 H27B 108.3 . . ?
C5 N28 Cu5 109.5(6) . . ?
C5 N28 H28A 109.8 . . ?
Cu5 N28 H28A 109.8 . . ?
C5 N28 H28B 109.8 . . ?
Cu5 N28 H28B 109.8 . . ?
H28A N28 H28B 108.2 . . ?
H1WA O1W H1WB 104.5 . . ?
N30 N31 Cu1 123.4(6) . . ?
N31 N30 N29 179.3(12) . . ?
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
Cu1 N1 1.943(6) . ?
Cu1 N31 1.962(6) . ?
Cu1 N7 2.004(6) . ?
Cu1 N4 2.021(5) . ?
Cu2 N10 1.985(5) . ?
Cu2 N7 1.992(5) . ?
Cu2 N13 1.998(5) . ?
Cu2 N4 2.009(5) . ?
Cu3 N19 2.004(6) . ?
Cu3 N10 2.012(6) . ?
Cu3 N20 2.012(5) . ?
Cu3 N16 2.015(6) . ?
Cu4 N24 1.960(6) . ?
Cu4 N16 1.987(6) . ?
Cu4 N21 2.009(6) 2_677 ?
Cu4 N21 2.028(6) . ?
Cu5 N27 2.001(7) 2_676 ?
Cu5 N27 2.001(7) . ?
Cu5 N28 2.010(7) . ?
Cu5 N28 2.010(7) 2_676 ?
C1 C2 1.481(10) . ?
C1 N19 1.484(9) . ?
C1 C3' 1.514(16) . ?
C1 H1A 0.9600 . ?
C2 N20 1.488(10) . ?
C2 C3 1.5000(11) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C3 H2A 0.5413 . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C3' H3'1 0.9600 . ?
C3' H3'2 0.9600 . ?
C3' H3'3 0.9600 . ?
C4 C5 1.434(5) . ?
C4 N27 1.434(11) . ?
C4 C6 1.506(13) . ?
C4 H4 0.9799 . ?
C5 N28 1.435(12) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9601 . ?
N1 N2 1.179(8) . ?
N2 N3 1.169(8) . ?
N4 N5 1.190(8) . ?
N5 N6 1.132(8) . ?
N7 N8 1.210(8) . ?
N8 N9 1.117(8) . ?
N10 N11 1.178(8) . ?
N11 N12 1.144(8) . ?
N13 N14 1.193(8) . ?
N14 N15 1.105(9) . ?
N16 N17 1.203(8) . ?
N17 N18 1.122(9) . ?
N19 H19A 0.9000 . ?
N19 H19B 0.9000 . ?
N20 H20A 0.9000 . ?
N20 H20B 0.9000 . ?
N21 N22 1.198(8) . ?
N21 Cu4 2.009(6) 2_677 ?
N22 N23 1.119(8) . ?
N24 N25 1.165(9) . ?
N25 N26 1.128(10) . ?
N27 H27A 0.9000 . ?
N27 H27B 0.9000 . ?
N28 H28A 0.9000 . ?
N28 H28B 0.9000 . ?
O1W H1WA 0.8500 . ?
O1W H1WB 0.8500 . ?
N31 N30 1.129(9) . ?
N30 N29 1.140(13) . ?
