#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/82/7008235.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_7008235
loop_
_publ_author_name
'Zhao, Wei'
'Fan, Jian'
'Song, You'
'Kawaguchi, Hiroyuki'
'Okamura, Taka-aki'
'Sun, Wei-Yin'
'Ueyama, Norikazu'
_publ_section_title
;
 Syntheses, crystal structures and properties of novel copper(II)
 complexes obtained by reactions of copper(II) sulfate pentahydrate
 with tripodal ligands.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1509
_journal_page_last               1517
_journal_paper_doi               10.1039/b419418g
_journal_year                    2005
_chemical_formula_moiety         'C17 H29 Cu N6 O10.50 S '
_chemical_formula_sum            'C17 H29 Cu N6 O10.5 S'
_chemical_formula_weight         581.06
_chemical_name_common            (Cu(3)(H2O))SO4-5.5(H2O)
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_date             'Thu Feb 3 21:43:02 2005'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                83.533(17)
_cell_angle_beta                 86.67(3)
_cell_angle_gamma                83.22(3)
_cell_formula_units_Z            2
_cell_length_a                   8.010(5)
_cell_length_b                   11.542(4)
_cell_length_c                   13.090(5)
_cell_measurement_reflns_used    3207
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.6
_cell_measurement_theta_min      3.1
_cell_volume                     1192.8(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      200
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0927
_diffrn_reflns_av_sigmaI/netI    0.1781
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11788
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.07
_exptl_absorpt_coefficient_mu    1.070
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.618
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             604
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.764
_refine_diff_density_min         -0.547
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.830
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         5395
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.830
_refine_ls_R_factor_all          0.0778
_refine_ls_R_factor_gt           0.0529
_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)+(0.0000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1233
_refine_ls_wR_factor_ref         0.1449
_reflns_number_gt                3135
_reflns_number_total             5395
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            b419418g.txt
_cod_data_source_block           6
_cod_original_cell_volume        1192.8(9)
_cod_original_formula_sum        'C17 H29 Cu N6 O10.50 S'
_cod_database_code               7008235
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 0.0000 1.0000 0.0000 0.02370(19) Uani 1 2 d S . .
Cu2 Cu 0.0000 0.5000 0.5000 0.02416(19) Uani 1 2 d S . .
S1 S 0.20509(13) 0.86308(8) 0.23095(7) 0.0244(2) Uani 1 1 d . . .
O1 O 0.2466(3) 1.0165(2) -0.01027(18) 0.0258(6) Uani 1 1 d . . .
H1 H 0.2994 0.9871 0.0498 0.031 Uiso 1 1 d . . .
H2 H 0.3087 0.9639 -0.0602 0.026 Uiso 1 1 d . . .
O2 O 0.1962(4) 0.6517(2) 0.46225(19) 0.0376(7) Uani 1 1 d . . .
O3 O 0.4257(4) 0.9285(2) 0.82720(19) 0.0351(7) Uani 1 1 d . . .
O4 O 0.4991(5) 0.9060(3) 0.4410(2) 0.0584(10) Uani 1 1 d . . .
O5 O 0.2104(5) 0.0231(3) 0.6700(2) 0.0606(10) Uani 1 1 d . . .
O6 O 0.6678(5) 0.2325(3) 0.3920(3) 0.0660(11) Uani 1 1 d . . .
O7 O 0.0437(14) 0.9764(12) 0.5109(12) 0.093(4) Uani 0.50 1 d P . .
O11 O 0.3440(4) 0.9166(2) 0.1711(2) 0.0381(7) Uani 1 1 d . . .
O12 O 0.0436(3) 0.9077(2) 0.18211(19) 0.0272(6) Uani 1 1 d . . .
O13 O 0.2000(5) 0.8915(3) 0.3371(2) 0.0589(10) Uani 1 1 d . . .
O14 O 0.2340(4) 0.7352(2) 0.2292(2) 0.0424(8) Uani 1 1 d . . .
N11 N 0.1357(4) 0.6592(2) -0.0640(2) 0.0233(7) Uani 1 1 d . . .
N12 N 0.0448(4) 0.8452(2) -0.0541(2) 0.0240(7) Uani 1 1 d . . .
N31 N 0.3172(4) 0.3546(2) 0.2725(2) 0.0229(7) Uani 1 1 d . . .
N32 N 0.1289(4) 0.4062(3) 0.3941(2) 0.0258(7) Uani 1 1 d . . .
N51 N 0.2718(4) 0.3112(2) -0.2611(2) 0.0220(7) Uani 1 1 d . . .
N52 N 0.1586(4) 0.4150(3) -0.3969(2) 0.0242(7) Uani 1 1 d . . .
C1 C 0.2084(5) 0.5423(3) -0.0353(3) 0.0210(8) Uani 1 1 d . . .
C2 C 0.2837(5) 0.5125(3) 0.0586(3) 0.0224(8) Uani 1 1 d . . .
H3 H 0.2848 0.5697 0.1052 0.027 Uiso 1 1 calc R . .
C3 C 0.3581(5) 0.3975(3) 0.0839(3) 0.0211(8) Uani 1 1 d . . .
C4 C 0.3570(5) 0.3146(3) 0.0149(3) 0.0235(8) Uani 1 1 d . . .
H4 H 0.4077 0.2367 0.0321 0.028 Uiso 1 1 calc R . .
C5 C 0.2823(5) 0.3449(3) -0.0794(2) 0.0230(9) Uani 1 1 d . . .
C6 C 0.2069(5) 0.4578(3) -0.1039(3) 0.0238(9) Uani 1 1 d . . .
H5 H 0.1539 0.4782 -0.1675 0.029 Uiso 1 1 calc R . .
C12 C 0.1189(5) 0.7497(3) -0.0051(3) 0.0284(10) Uani 1 1 d . . .
H6 H 0.1562 0.7444 0.0630 0.034 Uiso 1 1 calc R . .
C13 C 0.0103(6) 0.8174(3) -0.1488(3) 0.0323(10) Uani 1 1 d . . .
H7 H -0.0432 0.8699 -0.2013 0.039 Uiso 1 1 calc R . .
C14 C 0.0646(6) 0.7033(3) -0.1558(3) 0.0378(12) Uani 1 1 d . . .
H8 H 0.0556 0.6612 -0.2132 0.045 Uiso 1 1 calc R . .
C31 C 0.4409(5) 0.3659(3) 0.1857(2) 0.0231(8) Uani 1 1 d . . .
H9 H 0.5141 0.2908 0.1836 0.028 Uiso 1 1 calc R . .
H10 H 0.5128 0.4272 0.1964 0.028 Uiso 1 1 calc R . .
C32 C 0.2330(5) 0.4446(3) 0.3198(3) 0.0291(9) Uani 1 1 d . . .
H11 H 0.2474 0.5250 0.3016 0.035 Uiso 1 1 calc R . .
C33 C 0.1486(6) 0.2843(3) 0.3963(3) 0.0310(10) Uani 1 1 d . . .
H12 H 0.0901 0.2316 0.4422 0.037 Uiso 1 1 calc R . .
C34 C 0.2652(6) 0.2535(3) 0.3219(3) 0.0313(10) Uani 1 1 d . . .
H13 H 0.3037 0.1759 0.3069 0.038 Uiso 1 1 calc R . .
C51 C 0.2826(5) 0.2541(3) -0.1568(2) 0.0223(8) Uani 1 1 d . . .
H14 H 0.3871 0.1992 -0.1514 0.027 Uiso 1 1 calc R . .
H15 H 0.1859 0.2082 -0.1400 0.027 Uiso 1 1 calc R . .
C52 C 0.1279(5) 0.3500(3) -0.3097(3) 0.0209(8) Uani 1 1 d . . .
H16 H 0.0190 0.3328 -0.2844 0.025 Uiso 1 1 calc R . .
C53 C 0.3299(6) 0.4164(4) -0.4056(3) 0.0343(10) Uani 1 1 d . . .
H17 H 0.3899 0.4552 -0.4614 0.041 Uiso 1 1 calc R . .
C54 C 0.4007(5) 0.3528(3) -0.3210(3) 0.0301(9) Uani 1 1 d . . .
H18 H 0.5169 0.3403 -0.3069 0.036 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
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
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
N12 Cu1 N12 180.00(15) . 2_575 ?
N12 Cu1 O1 90.23(12) . . ?
N12 Cu1 O1 89.77(12) 2_575 . ?
N12 Cu1 O1 89.77(12) . 2_575 ?
N12 Cu1 O1 90.23(12) 2_575 2_575 ?
O1 Cu1 O1 180.0 . 2_575 ?
N52 Cu2 N52 180.00(15) 2_565 1_556 ?
N52 Cu2 N32 92.68(12) 2_565 . ?
N52 Cu2 N32 87.32(12) 1_556 . ?
N52 Cu2 N32 87.32(12) 2_565 2_566 ?
N52 Cu2 N32 92.68(12) 1_556 2_566 ?
N32 Cu2 N32 179.998(1) . 2_566 ?
O13 S1 O14 109.7(2) . . ?
O13 S1 O11 109.84(18) . . ?
O14 S1 O11 108.67(19) . . ?
O13 S1 O12 110.61(18) . . ?
O14 S1 O12 108.91(15) . . ?
O11 S1 O12 109.09(17) . . ?
Cu1 O1 H1 112.0 . . ?
Cu1 O1 H2 111.0 . . ?
H1 O1 H2 100.0 . . ?
C12 N11 C14 105.8(3) . . ?
C12 N11 C1 126.7(3) . . ?
C14 N11 C1 127.4(3) . . ?
C12 N12 C13 106.7(3) . . ?
C12 N12 Cu1 125.5(2) . . ?
C13 N12 Cu1 127.8(2) . . ?
C32 N31 C34 106.7(3) . . ?
C32 N31 C31 125.9(3) . . ?
C34 N31 C31 127.4(3) . . ?
C32 N32 C33 105.9(3) . . ?
C32 N32 Cu2 127.1(3) . . ?
C33 N32 Cu2 126.2(3) . . ?
C52 N51 C54 107.3(3) . . ?
C52 N51 C51 125.8(3) . . ?
C54 N51 C51 126.1(3) . . ?
C52 N52 C53 105.9(3) . . ?
C52 N52 Cu2 130.2(3) . 1_554 ?
C53 N52 Cu2 123.9(3) . 1_554 ?
C2 C1 C6 120.1(3) . . ?
C2 C1 N11 120.7(3) . . ?
C6 C1 N11 119.2(3) . . ?
C1 C2 C3 119.6(3) . . ?
C1 C2 H3 120.2 . . ?
C3 C2 H3 120.2 . . ?
C4 C3 C2 119.8(3) . . ?
C4 C3 C31 120.9(3) . . ?
C2 C3 C31 119.3(3) . . ?
C3 C4 C5 120.5(3) . . ?
C3 C4 H4 119.7 . . ?
C5 C4 H4 119.7 . . ?
C6 C5 C4 119.7(3) . . ?
C6 C5 C51 119.5(3) . . ?
C4 C5 C51 120.8(3) . . ?
C5 C6 C1 120.3(3) . . ?
C5 C6 H5 119.9 . . ?
C1 C6 H5 119.9 . . ?
N12 C12 N11 111.3(3) . . ?
N12 C12 H6 124.3 . . ?
N11 C12 H6 124.3 . . ?
C14 C13 N12 109.0(3) . . ?
C14 C13 H7 125.5 . . ?
N12 C13 H7 125.5 . . ?
C13 C14 N11 107.1(3) . . ?
C13 C14 H8 126.4 . . ?
N11 C14 H8 126.4 . . ?
N31 C31 C3 112.2(3) . . ?
N31 C31 H9 109.2 . . ?
C3 C31 H9 109.2 . . ?
N31 C31 H10 109.2 . . ?
C3 C31 H10 109.2 . . ?
H9 C31 H10 107.9 . . ?
N32 C32 N31 111.4(3) . . ?
N32 C32 H11 124.3 . . ?
N31 C32 H11 124.3 . . ?
C34 C33 N32 108.6(4) . . ?
C34 C33 H12 125.7 . . ?
N32 C33 H12 125.7 . . ?
C33 C34 N31 107.4(3) . . ?
C33 C34 H13 126.3 . . ?
N31 C34 H13 126.3 . . ?
N51 C51 C5 110.9(3) . . ?
N51 C51 H14 109.5 . . ?
C5 C51 H14 109.5 . . ?
N51 C51 H15 109.5 . . ?
C5 C51 H15 109.5 . . ?
H14 C51 H15 108.0 . . ?
N52 C52 N51 111.2(4) . . ?
N52 C52 H16 124.4 . . ?
N51 C52 H16 124.4 . . ?
C54 C53 N52 109.2(4) . . ?
C54 C53 H17 125.4 . . ?
N52 C53 H17 125.4 . . ?
N51 C54 C53 106.4(4) . . ?
N51 C54 H18 126.8 . . ?
C53 C54 H18 126.8 . . ?
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 N12 1.981(3) . ?
Cu1 N12 1.981(3) 2_575 ?
Cu1 O1 2.002(3) . ?
Cu1 O1 2.002(3) 2_575 ?
Cu2 N52 2.001(3) 2_565 ?
Cu2 N52 2.001(3) 1_556 ?
Cu2 N32 2.017(3) . ?
Cu2 N32 2.017(3) 2_566 ?
S1 O13 1.461(3) . ?
S1 O14 1.469(3) . ?
S1 O11 1.478(3) . ?
S1 O12 1.487(3) . ?
O1 H1 0.9300 . ?
O1 H2 1.0100 . ?
O7 O7 0.876(17) 2_576 ?
N11 C12 1.356(4) . ?
N11 C14 1.378(5) . ?
N11 C1 1.424(4) . ?
N12 C12 1.307(5) . ?
N12 C13 1.366(4) . ?
N31 C32 1.360(4) . ?
N31 C34 1.367(5) . ?
N31 C31 1.468(4) . ?
N32 C32 1.316(5) . ?
N32 C33 1.395(4) . ?
N51 C52 1.354(5) . ?
N51 C54 1.360(5) . ?
N51 C51 1.451(4) . ?
N52 C52 1.320(4) . ?
N52 C53 1.372(5) . ?
N52 Cu2 2.001(3) 1_554 ?
C1 C2 1.390(5) . ?
C1 C6 1.400(4) . ?
C2 C3 1.401(5) . ?
C2 H3 0.9500 . ?
C3 C4 1.388(4) . ?
C3 C31 1.511(5) . ?
C4 C5 1.394(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.381(5) . ?
C5 C51 1.536(4) . ?
C6 H5 0.9500 . ?
C12 H6 0.9500 . ?
C13 C14 1.349(5) . ?
C13 H7 0.9500 . ?
C14 H8 0.9500 . ?
C31 H9 0.9900 . ?
C31 H10 0.9900 . ?
C32 H11 0.9500 . ?
C33 C34 1.357(5) . ?
C33 H12 0.9500 . ?
C34 H13 0.9500 . ?
C51 H14 0.9900 . ?
C51 H15 0.9900 . ?
C52 H16 0.9500 . ?
C53 C54 1.370(5) . ?
C53 H17 0.9500 . ?
C54 H18 0.9500 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 Cu1 N12 C12 69.7(4) . . . . ?
O1 Cu1 N12 C12 -110.3(4) 2_575 . . . ?
O1 Cu1 N12 C13 -108.2(3) . . . . ?
O1 Cu1 N12 C13 71.8(3) 2_575 . . . ?
N52 Cu2 N32 C32 72.7(3) 2_565 . . . ?
N52 Cu2 N32 C32 -107.3(3) 1_556 . . . ?
N52 Cu2 N32 C33 -119.5(3) 2_565 . . . ?
N52 Cu2 N32 C33 60.5(3) 1_556 . . . ?
C12 N11 C1 C2 -5.1(6) . . . . ?
C14 N11 C1 C2 176.5(4) . . . . ?
C12 N11 C1 C6 176.4(4) . . . . ?
C14 N11 C1 C6 -2.0(6) . . . . ?
C6 C1 C2 C3 0.1(6) . . . . ?
N11 C1 C2 C3 -178.4(4) . . . . ?
C1 C2 C3 C4 0.5(6) . . . . ?
C1 C2 C3 C31 179.5(3) . . . . ?
C2 C3 C4 C5 -0.1(6) . . . . ?
C31 C3 C4 C5 -179.2(4) . . . . ?
C3 C4 C5 C6 -0.7(6) . . . . ?
C3 C4 C5 C51 179.2(4) . . . . ?
C4 C5 C6 C1 1.3(6) . . . . ?
C51 C5 C6 C1 -178.7(3) . . . . ?
C2 C1 C6 C5 -0.9(6) . . . . ?
N11 C1 C6 C5 177.6(4) . . . . ?
C13 N12 C12 N11 0.3(5) . . . . ?
Cu1 N12 C12 N11 -178.1(3) . . . . ?
C14 N11 C12 N12 -0.6(5) . . . . ?
C1 N11 C12 N12 -179.3(4) . . . . ?
C12 N12 C13 C14 0.2(5) . . . . ?
Cu1 N12 C13 C14 178.4(3) . . . . ?
N12 C13 C14 N11 -0.5(5) . . . . ?
C12 N11 C14 C13 0.6(5) . . . . ?
C1 N11 C14 C13 179.3(4) . . . . ?
C32 N31 C31 C3 -81.0(4) . . . . ?
C34 N31 C31 C3 99.7(4) . . . . ?
C4 C3 C31 N31 -105.9(4) . . . . ?
C2 C3 C31 N31 75.0(4) . . . . ?
C33 N32 C32 N31 1.0(4) . . . . ?
Cu2 N32 C32 N31 170.7(2) . . . . ?
C34 N31 C32 N32 -1.5(4) . . . . ?
C31 N31 C32 N32 179.1(3) . . . . ?
C32 N32 C33 C34 -0.2(4) . . . . ?
Cu2 N32 C33 C34 -170.0(3) . . . . ?
N32 C33 C34 N31 -0.7(5) . . . . ?
C32 N31 C34 C33 1.3(4) . . . . ?
C31 N31 C34 C33 -179.3(3) . . . . ?
C52 N51 C51 C5 -88.9(4) . . . . ?
C54 N51 C51 C5 79.1(4) . . . . ?
C6 C5 C51 N51 26.1(5) . . . . ?
C4 C5 C51 N51 -153.8(4) . . . . ?
C53 N52 C52 N51 1.0(4) . . . . ?
Cu2 N52 C52 N51 -178.16(19) 1_554 . . . ?
C54 N51 C52 N52 -0.5(4) . . . . ?
C51 N51 C52 N52 169.4(3) . . . . ?
C52 N52 C53 C54 -1.1(4) . . . . ?
Cu2 N52 C53 C54 178.1(2) 1_554 . . . ?
C52 N51 C54 C53 -0.2(4) . . . . ?
C51 N51 C54 C53 -170.1(3) . . . . ?
N52 C53 C54 N51 0.8(4) . . . . ?
