#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/21/4322154.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_4322154
loop_
_publ_author_name
'Yoshiki Shii'
'Yuri Motoda'
'Toshihiro Matsuo'
'Fumiaki Kai'
'Toshio Nakashima'
'Jean-Pierre Tuchagues'
'Naohide Matsumoto'
_publ_contact_author
;
Naohide Matsumoto
 Department of Chemistry, Faculty of Science, Kumamoto University,
Kurokami 2-39-1, Kumamoto 860-8555, Japan
;
_publ_contact_author_email       'naohide@aster.sci.kumamoto-u.ac.jp '
_publ_contact_author_fax         +81-96-342-3390
_publ_contact_author_phone       ' +81-96-342-3390'
_publ_section_title
;
 Deprotonation-Induced Enantioselective Aggregation and
 Deprotonation-Induced Ligand Rearrangement of Copper(II) Complexes Yield
 1D Homochiral and Heterochiral Chains and a Cyclic Tetramer, Respectively
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3513
_journal_page_last               3522
_journal_paper_doi               10.1021/ic9813260
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C15 H30 Cl Cu N7 O8'
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      88
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_audit_creation_date             'Wed Dec 24 15:51:19 1997'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16.00
_cell_length_a                   17.318(3)
_cell_length_b                   17.3177
_cell_length_c                   30.432(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    20.0
_cell_measurement_theta_max      26.06
_cell_measurement_theta_min      20.05
_cell_volume                     9127(2)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan: PROCESS (MSC)'
_computing_publication_material  'teXsan: FINISH (MSC)'
_computing_structure_refinement  'teXsan: LS (MSC)'
_computing_structure_solution    SAPI91
_diffrn_ambient_temperature      20.0
_diffrn_measurement_device       AFC7R
_diffrn_measurement_method       'omega/2-theta scans'
_diffrn_orient_matrix_UB_11      -0.02751
_diffrn_orient_matrix_UB_12      -0.04574
_diffrn_orient_matrix_UB_13      -0.01254
_diffrn_orient_matrix_UB_21      -0.04931
_diffrn_orient_matrix_UB_22      0.03003
_diffrn_orient_matrix_UB_23      -0.00045
_diffrn_orient_matrix_UB_31      0.01208
_diffrn_orient_matrix_UB_32      0.01844
_diffrn_orient_matrix_UB_33      -0.03037
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoKalpha
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  6.02
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4409
_diffrn_reflns_theta_max         24.9934
_diffrn_standards_decay_%        -1.11
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu_cm 11.255
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.970
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.559
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             4464.00
_exptl_crystal_size_max          0.300
_exptl_crystal_size_min          0.200
_refine_diff_density_max         -0.51200
_refine_diff_density_min         0.52370
_refine_ls_extinction_coef       0.00000
_refine_ls_extinction_method     Zachariasen_type_2_Gaussian_isotropic
_refine_ls_goodness_of_fit_obs   1.770
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         1876
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0830
_refine_ls_shift/esd_max         1.1440
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_obs         0.0560
_cod_data_source_file            ic9813260_5.cif
_cod_data_source_block           Cu_(2_3)Me'
_cod_original_cell_volume        9126(1)
_cod_original_sg_symbol_H-M      'I 41/a '
_cod_original_formula_sum        'C15 H30 N7 O8 Cl Cu'
_cod_database_code               4322154
loop_
_symmetry_equiv_pos_as_xyz
'   +x,   +y,   +z'
1/2+x,1/2+y,1/2+z
'   -x,1/2-y,   +z'
'1/2-x,   -y,1/2+z'
3/4-y,1/4+x,1/4+z
1/4-y,3/4+x,3/4+z
1/4+y,1/4-x,1/4+z
3/4+y,3/4-x,3/4+z
'   -x,   -y,   -z'
' 1/2-x,1/2-y,1/2-z'
'   +x,1/2+y,   -z'
'1/2+x,   +y,1/2-z'
3/4+y,1/4-x,1/4-z
1/4+y,3/4-x,3/4-z
1/4-y,1/4+x,1/4-z
3/4-y,3/4+x,3/4-z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_calc_attached_atom
Cu1 0.15166(8) 0.06708(8) 0.65429(4) 0.0402(4) Uij ? ?
Cl1 0.7008(4) 0.2005(3) 0.0517(2) 0.120(2) Uij ? ?
O1 0.6794(9) 0.2754(7) 0.0415(4) 0.166(7) Uij ? ?
O2 0.626(2) 0.163(1) 0.060(1) 0.40(2) Uij ? ?
O3 0.740(1) 0.2002(10) 0.0892(5) 0.27(1) Uij ? ?
O4 0.740(2) 0.167(1) 0.0218(5) 0.38(2) Uij ? ?
O5 1.0037(4) 0.0335(5) 0.0421(3) 0.065(3) Uij ? ?
O6 0.0734(9) 0.1796(10) 0.1983(6) 0.246(10) Uij ? ?
O7 0.596(1) 0.219(1) 0.7130(7) 0.31(1) Uij ? ?
O8 1.0000 0.2500 0.1250 0.52(3) Uij ? ?
N1 0.2350(5) 0.0109(5) 0.6107(3) 0.039(3) Uij ? ?
N2 0.3404(6) -0.0401(6) 0.5836(3) 0.052(4) Uij ? ?
N3 0.1700(6) -0.1775(6) 0.6558(4) 0.069(4) Uij ? ?
N4 0.1530(5) -0.0456(5) 0.6817(3) 0.042(3) Uij ? ?
N5 0.2083(5) 0.0925(6) 0.7087(3) 0.041(3) Uij ? ?
N6 0.1930(5) 0.3029(5) 0.6274(3) 0.034(3) Uij ? ?
N7 0.1719(5) 0.1799(5) 0.6435(3) 0.034(3) Uij ? ?
C1 0.3275(7) 0.1045(9) 0.5772(4) 0.072(5) Uij ? ?
C2 0.3008(7) 0.0252(7) 0.5904(4) 0.046(4) Uij ? ?
C3 0.2978(8) -0.0991(7) 0.6018(4) 0.060(5) Uij ? ?
C4 0.2340(7) -0.0675(7) 0.6186(4) 0.041(4) Uij ? ?
C5 0.1654(7) -0.0972(6) 0.6423(4) 0.046(4) Uij ? ?
C6 0.0954(9) -0.2022(8) 0.6734(5) 0.085(6) Uij ? ?
C7 0.0767(8) -0.1553(8) 0.7142(5) 0.077(6) Uij ? ?
C8 0.0790(7) -0.0690(8) 0.7034(4) 0.066(5) Uij ? ?
C9 0.2192(7) -0.0448(7) 0.7134(4) 0.046(4) Uij ? ?
C10 0.2190(7) 0.0314(7) 0.7397(4) 0.050(4) Uij ? ?
C11 0.2366(6) 0.1598(6) 0.7114(3) 0.038(4) Uij ? ?
C12 0.2157(6) 0.2103(7) 0.6770(3) 0.038(4) Uij ? ?
C13 0.2275(7) 0.2853(7) 0.6662(4) 0.042(4) Uij ? ?
C14 0.1577(6) 0.2360(7) 0.6150(3) 0.035(4) Uij ? ?
C15 0.1142(7) 0.2290(7) 0.5738(4) 0.058(5) Uij ? ?
H1 0.3765 0.1113 0.5902 0.0710 Uij ? ?
H2 0.3356 0.1008 0.5452 0.0710 Uij ? ?
H3 0.2917 0.1382 0.5842 0.0785 Uij ? ?
H4 0.3900 -0.0452 0.5688 0.0907 Uij ? ?
H5 0.3142 -0.1530 0.6022 0.0820 Uij ? ?
H6 0.1034 -0.0846 0.6250 0.0763 Uij ? ?
H7 0.2151 -0.2086 0.6528 0.0622 Uij ? ?
H8 0.0573 -0.1926 0.6539 0.0907 Uij ? ?
H9 0.0999 -0.2537 0.6822 0.0907 Uij ? ?
H10 0.0292 -0.1699 0.7259 0.0879 Uij ? ?
H11 0.1165 -0.1654 0.7372 0.0879 Uij ? ?
H12 0.0715 -0.0408 0.7285 0.0720 Uij ? ?
H13 0.0382 -0.0614 0.6827 0.0720 Uij ? ?
H14 0.2131 -0.0892 0.7330 0.0521 Uij ? ?
H15 0.2664 -0.0519 0.6980 0.0521 Uij ? ?
H16 0.1782 0.0280 0.7602 0.0534 Uij ? ?
H17 0.2670 0.0341 0.7543 0.0534 Uij ? ?
H18 0.2684 0.1742 0.7348 0.0541 Uij ? ?
H19 0.2584 0.3208 0.6825 0.0613 Uij ? ?
H20 0.1127 0.2777 0.5598 0.0794 Uij ? ?
H21 0.0647 0.2113 0.5804 0.0621 Uij ? ?
H22 0.1404 0.1929 0.5551 0.0621 Uij ? ?
loop_
_atom_type_symbol
_atom_type_oxidation_number
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 0 240 0.003 0.002 'International Tables'
H 0 480 0.000 0.000 'International Tables'
N 0 112 0.006 0.003 'International Tables'
Cl 0 16 0.148 0.159 'International Tables'
O 0 128 0.011 0.006 'International Tables'
Cu 0 16 0.320 1.265 'International Tables'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
? ? ?
? ? ?
? ? ?
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N(1) Cu(1) N(4) 79.8(3) ? ? ? yes
N(1) Cu(1) N(5) 106.3(3) ? ? ? yes
N(1) Cu(1) N(6) 103.7(3) ? ? ? yes
N(1) Cu(1) N(7) 102.6(3) ? ? ? yes
N(4) Cu(1) N(5) 82.5(4) ? ? ? yes
N(4) Cu(1) N(6) 96.9(4) ? ? ? yes
N(4) Cu(1) N(7) 162.7(3) ? ? ? yes
N(5) Cu(1) N(6) 149.4(4) ? ? ? yes
N(5) Cu(1) N(7) 80.4(4) ? ? ? yes
N(6) Cu(1) N(7) 99.0(3) ? ? ? yes
O(1) Cl(1) O(2) 102(1) ? ? ? yes
O(1) Cl(1) O(3) 109.4(10) ? ? ? yes
O(1) Cl(1) O(4) 114(1) ? ? ? yes
O(2) Cl(1) O(3) 107(1) ? ? ? yes
O(2) Cl(1) O(4) 112(1) ? ? ? yes
O(3) Cl(1) O(4) 110(1) ? ? ? yes
Cu(1) N(1) C(2) 140.4(9) ? ? ? yes
Cu(1) N(1) C(4) 108.9(8) ? ? ? yes
C(2) N(1) C(4) 106.0(10) ? ? ? yes
C(2) N(2) C(3) 106(1) ? ? ? yes
C(5) N(3) C(6) 109(1) ? ? ? yes
Cu(1) N(4) C(5) 103.5(6) ? ? ? yes
Cu(1) N(4) C(8) 114.4(7) ? ? ? yes
Cu(1) N(4) C(9) 104.6(7) ? ? ? yes
C(5) N(4) C(8) 108.1(9) ? ? ? yes
C(5) N(4) C(9) 114.1(9) ? ? ? yes
C(8) N(4) C(9) 112.0(9) ? ? ? yes
Cu(1) N(5) C(10) 116.9(8) ? ? ? yes
Cu(1) N(5) C(11) 116.8(8) ? ? ? yes
C(10) N(5) C(11) 126(1) ? ? ? yes
Cu(1) N(6) C(13) 131.2(8) ? ? ? yes
Cu(1) N(6) C(14) 124.2(7) ? ? ? yes
C(13) N(6) C(14) 104.3(9) ? ? ? yes
Cu(1) N(7) C(12) 110.3(7) ? ? ? yes
Cu(1) N(7) C(14) 141.8(8) ? ? ? yes
C(12) N(7) C(14) 107.9(9) ? ? ? yes
N(1) C(2) N(2) 110(1) ? ? ? yes
N(1) C(2) C(1) 124(1) ? ? ? yes
N(2) C(2) C(1) 124(1) ? ? ? yes
N(2) C(3) C(4) 107(1) ? ? ? yes
N(1) C(4) C(3) 109(1) ? ? ? yes
N(1) C(4) C(5) 115(1) ? ? ? yes
C(3) C(4) C(5) 135(1) ? ? ? yes
N(3) C(5) N(4) 110.4(9) ? ? ? yes
N(3) C(5) C(4) 115(1) ? ? ? yes
N(4) C(5) C(4) 107.1(9) ? ? ? yes
N(3) C(6) C(7) 109(1) ? ? ? yes
C(6) C(7) C(8) 109(1) ? ? ? yes
N(4) C(8) C(7) 112(1) ? ? ? yes
N(4) C(9) C(10) 109.9(9) ? ? ? yes
N(5) C(10) C(9) 107.0(9) ? ? ? yes
N(5) C(11) C(12) 115(1) ? ? ? yes
N(7) C(12) C(11) 116(1) ? ? ? yes
N(7) C(12) C(13) 105.7(9) ? ? ? yes
C(11) C(12) C(13) 137(1) ? ? ? yes
N(6) C(13) C(12) 111(1) ? ? ? yes
N(6) C(14) N(7) 111.0(9) ? ? ? yes
N(6) C(14) C(15) 122(1) ? ? ? yes
N(7) C(14) C(15) 126(1) ? ? ? yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu(1) N(1) 2.189(9) ? ? yes
Cu(1) N(4) 2.123(9) ? ? yes
Cu(1) N(5) 1.975(9) ? ? yes
Cu(1) N(6) 1.972(9) ? ? yes
Cu(1) N(7) 2.012(8) ? ? yes
Cl(1) O(1) 1.38(1) ? ? yes
Cl(1) O(2) 1.47(2) ? ? yes
Cl(1) O(3) 1.32(1) ? ? yes
Cl(1) O(4) 1.27(2) ? ? yes
N(1) C(2) 1.32(1) ? ? yes
N(1) C(4) 1.38(1) ? ? yes
N(2) C(2) 1.34(1) ? ? yes
N(2) C(3) 1.38(1) ? ? yes
N(3) C(5) 1.45(1) ? ? yes
N(3) C(6) 1.46(2) ? ? yes
N(4) C(5) 1.51(1) ? ? yes
N(4) C(8) 1.50(1) ? ? yes
N(4) C(9) 1.50(1) ? ? yes
N(5) C(10) 1.43(1) ? ? yes
N(5) C(11) 1.27(1) ? ? yes
N(6) C(13) 1.36(1) ? ? yes
N(6) C(14) 1.36(1) ? ? yes
N(7) C(12) 1.37(1) ? ? yes
N(7) C(14) 1.33(1) ? ? yes
C(1) C(2) 1.50(2) ? ? yes
C(3) C(4) 1.33(2) ? ? yes
C(4) C(5) 1.48(1) ? ? yes
C(6) C(7) 1.52(2) ? ? yes
C(7) C(8) 1.53(2) ? ? yes
C(9) C(10) 1.54(1) ? ? yes
C(11) C(12) 1.41(1) ? ? yes
C(12) C(13) 1.35(1) ? ? yes
C(14) C(15) 1.47(1) ? ? yes
