#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/29/4322960.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_4322960
loop_
_publ_author_name
'Peter Comba'
'Andreas Fath'
'Trevor W. Hambley'
'Andreas Kühner'
'David T. Richens'
'Annette Vielfort'
_publ_section_title
;
 Helical Figure-of-Eight Loop Dicopper(I) Compounds: Syntheses,
 Structures, and Dynamics
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4389
_journal_page_last               4401
_journal_paper_doi               10.1021/ic980216q
_journal_volume                  37
_journal_year                    1998
_chemical_compound_source        -
_chemical_formula_analytical     -
_chemical_formula_moiety         -
_chemical_formula_structural     -
_chemical_formula_sum            'C32 H54 Cl2 Cu2 N4 O17 S4'
_chemical_formula_weight         1092.88
_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'
_audit_creation_date             'Fri Nov 17 13:55:20 1995'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                91.45(2)
_cell_angle_beta                 93.87(2)
_cell_angle_gamma                78.85(1)
_cell_formula_units_Z            2
_cell_length_a                   12.582(2)
_cell_length_b                   21.997(4)
_cell_length_c                   7.772(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294.2
_cell_measurement_theta_max      107.8
_cell_measurement_theta_min      97.2
_cell_volume                     2105.4(7)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    SHELXS-86
_diffrn_ambient_temperature      294.2
_diffrn_measurement_device       AFC7R
_diffrn_measurement_method       'omega/2-theta scans'
_diffrn_orient_matrix_UB_11      0.02416
_diffrn_orient_matrix_UB_12      -0.04598
_diffrn_orient_matrix_UB_13      0.00681
_diffrn_orient_matrix_UB_21      -0.01623
_diffrn_orient_matrix_UB_22      0.00165
_diffrn_orient_matrix_UB_23      0.12442
_diffrn_orient_matrix_UB_31      -0.07577
_diffrn_orient_matrix_UB_32      -0.00548
_diffrn_orient_matrix_UB_33      -0.03329
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           CuKalpha
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  1.97
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            6583
_diffrn_reflns_theta_max         60.00
_diffrn_standards_decay_%        5.48
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.767
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.598
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   psi-scan
_exptl_crystal_colour            clear
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_density_meas      ?
_exptl_crystal_description       needles
_exptl_crystal_F_000             1132
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.71
_refine_diff_density_min         -0.53
_refine_ls_extinction_coef       3.44073
_refine_ls_extinction_method     Zachariasen_type_2_Gaussian_isotropic
_refine_ls_goodness_of_fit_obs   4.376
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     554
_refine_ls_number_reflns         4749
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0619
_refine_ls_shift/esd_max         0.3290
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_obs         0.0685
_reflns_number_observed          4749
_reflns_number_total             6251
_reflns_observed_criterion       3.00
_cod_data_source_file            ic980216q_1.cif
_cod_data_source_block           bmh9
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value '-' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C32 H54 Cl2 Cu2 N4 O17 S4 '
_cod_database_code               4322960
loop_
_symmetry_equiv_pos_as_xyz
'   +x,   +y,   +z'
'   -x,   -y,   -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
Cu(1) 0.10868(9) 0.13986(4) 0.0085(1) 0.0524(3) Uij ? ?
Cu(2) 0.35671(8) 0.37426(5) -0.5136(1) 0.0480(3) Uij ? ?
Cl(1) 0.2410(2) 0.8640(1) 0.3981(3) 0.0675(7) Uij ? ?
Cl(2) 0.7923(2) 0.4157(1) 0.1083(3) 0.0697(7) Uij ? ?
S(1) -0.0542(2) 0.10424(9) 0.0690(2) 0.0561(6) Uij ? ?
S(2) 0.2116(2) 0.06559(9) 0.2073(2) 0.0589(6) Uij ? ?
S(3) 0.4807(2) 0.34448(9) -0.7325(2) 0.0577(6) Uij ? ?
S(4) 0.3582(2) 0.48193(8) -0.5582(2) 0.0544(6) Uij ? ?
O(1) 0.0952(4) 0.3832(2) -0.0558(7) 0.070(2) Uij ? ?
O(2) 0.4613(4) 0.2017(2) -0.0550(8) 0.073(2) Uij ? ?
O(3) -0.0236(4) 0.3105(2) -0.4069(7) 0.064(2) Uij ? ?
O(4) 0.3656(4) 0.1505(2) -0.4827(7) 0.057(2) Uij ? ?
O(5) 0.1275(5) 0.8738(3) 0.3469(8) 0.092(2) Uij ? ?
O(6) 0.258(2) 0.835(2) 0.556(3) 0.177(9) Uij ? ?
O(7) 0.298(2) 0.810(2) 0.301(6) 0.15(1) Uij ? ?
O(8) 0.286(2) 0.914(1) 0.383(8) 0.16(2) Uij ? ?
O(9) 0.7214(5) 0.4726(3) 0.1526(8) 0.084(2) Uij ? ?
O(10) 0.7396(8) 0.3677(4) 0.069(2) 0.206(6) Uij ? ?
O(11) 0.826(1) 0.4240(5) -0.060(1) 0.190(5) Uij ? ?
O(12) 0.887(1) 0.4073(7) 0.223(2) 0.219(6) Uij ? ?
O(13) 0.5000 0.0000 0.5000 1.11(2) Uij ? ?
O(15) 0.296(2) 0.875(5) 0.261(3) 0.22(2) Uij ? ?
O(16) 0.252(2) 0.913(2) 0.533(6) 0.13(1) Uij ? ?
O(17) 0.286(2) 0.809(1) 0.453(8) 0.09(2) Uij ? ?
O(18) 0.780(2) 0.382(1) 0.269(3) 0.122(7) Uij ? ?
O(19) 0.895(4) 0.412(2) 0.081(7) 0.28(2) Uij ? ?
N(1) 0.0466(4) 0.2236(2) 0.0875(7) 0.046(2) Uij ? ?
N(2) 0.1794(4) 0.0898(2) -0.1824(7) 0.045(2) Uij ? ?
N(3) 0.4727(4) 0.3393(2) -0.3400(7) 0.046(2) Uij ? ?
N(4) 0.1981(4) 0.3888(2) -0.5789(7) 0.044(2) Uij ? ?
C(1) -0.1258(6) 0.1827(4) 0.101(1) 0.060(2) Uij ? ?
C(2) -0.0541(6) 0.2266(3) 0.1775(9) 0.053(2) Uij ? ?
C(3) 0.0778(6) 0.2753(3) 0.0745(8) 0.045(2) Uij ? ?
C(4) 0.1808(6) 0.2814(3) 0.0060(8) 0.043(2) Uij ? ?
C(5) 0.2735(6) 0.2353(3) 0.0101(8) 0.044(2) Uij ? ?
C(6) 0.3672(5) 0.2445(3) -0.0550(9) 0.045(2) Uij ? ?
C(7) 0.3720(5) 0.3010(3) -0.1279(8) 0.045(2) Uij ? ?
C(8) 0.2822(6) 0.3485(3) -0.1316(8) 0.043(2) Uij ? ?
C(9) 0.1871(6) 0.3394(3) -0.0635(9) 0.047(2) Uij ? ?
C(10) 0.4727(6) 0.3094(3) -0.2014(9) 0.049(2) Uij ? ?
C(11) 0.5809(6) 0.3460(4) -0.3986(10) 0.060(3) Uij ? ?
C(12) 0.5940(6) 0.3186(4) -0.580(1) 0.067(3) Uij ? ?
C(13) 0.4999(7) 0.4201(4) -0.788(1) 0.070(3) Uij ? ?
C(14) 0.4002(8) 0.4722(4) -0.775(1) 0.073(3) Uij ? ?
C(15) 0.2111(6) 0.4997(3) -0.585(1) 0.064(3) Uij ? ?
C(16) 0.1599(6) 0.4490(3) -0.662(1) 0.061(2) Uij ? ?
C(17) 0.1287(5) 0.3549(3) -0.5641(8) 0.043(2) Uij ? ?
C(18) 0.1517(5) 0.2911(3) -0.5009(8) 0.039(2) Uij ? ?
C(19) 0.2531(6) 0.2522(3) -0.5214(8) 0.044(2) Uij ? ?
C(20) 0.2697(5) 0.1913(3) -0.4675(8) 0.041(2) Uij ? ?
C(21) 0.1888(5) 0.1693(3) -0.3881(8) 0.041(2) Uij ? ?
C(22) 0.0891(5) 0.2075(3) -0.3674(8) 0.045(2) Uij ? ?
C(23) 0.0703(5) 0.2689(3) -0.4236(8) 0.042(2) Uij ? ?
C(24) 0.2103(5) 0.1050(3) -0.3249(9) 0.043(2) Uij ? ?
C(25) 0.2025(7) 0.0241(3) -0.1380(9) 0.057(2) Uij ? ?
C(26) 0.2668(7) 0.0146(3) 0.0357(10) 0.061(3) Uij ? ?
C(27) 0.0998(7) 0.0315(3) 0.2737(10) 0.062(3) Uij ? ?
C(28) -0.0022(7) 0.0787(4) 0.2836(9) 0.059(3) Uij ? ?
C(29) 0.0795(7) 0.4367(4) -0.153(1) 0.067(3) Uij ? ?
C(30) 0.4619(7) 0.1396(4) -0.025(1) 0.073(3) Uij ? ?
C(31) -0.1119(6) 0.2925(4) -0.338(1) 0.068(3) Uij ? ?
C(32) 0.4581(6) 0.1736(3) -0.524(1) 0.067(3) Uij ? ?
H(1) -0.1639 0.2013 -0.0061 0.0701 Uij ? ?
H(2) -0.1887 0.1843 0.1775 0.0701 Uij ? ?
H(3) -0.0362 0.2144 0.2970 0.0643 Uij ? ?
H(4) -0.0942 0.2683 0.1793 0.0643 Uij ? ?
H(5) 0.0286 0.3121 0.1104 0.0530 Uij ? ?
H(6) 0.2719 0.1948 0.0614 0.0440 Uij ? ?
H(7) 0.2860 0.3886 -0.1798 0.0554 Uij ? ?
H(8) 0.5424 0.2917 -0.1391 0.0613 Uij ? ?
H(9) 0.5907 0.3885 -0.4031 0.0757 Uij ? ?
H(10) 0.6412 0.3250 -0.3211 0.0757 Uij ? ?
H(11) 0.6052 0.2738 -0.5639 0.0668 Uij ? ?
H(12) 0.6608 0.3267 -0.6187 0.0668 Uij ? ?
H(13) 0.5559 0.4313 -0.7142 0.0761 Uij ? ?
H(14) 0.5220 0.4180 -0.9049 0.0761 Uij ? ?
H(15) 0.3444 0.4610 -0.8552 0.0864 Uij ? ?
H(16) 0.4191 0.5089 -0.8188 0.0864 Uij ? ?
H(17) 0.1812 0.5073 -0.4675 0.0724 Uij ? ?
H(18) 0.1854 0.5371 -0.6451 0.0724 Uij ? ?
H(19) 0.1770 0.4459 -0.7834 0.0725 Uij ? ?
H(20) 0.0813 0.4602 -0.6635 0.0725 Uij ? ?
H(21) 0.0536 0.3708 -0.6032 0.0547 Uij ? ?
H(22) 0.3072 0.2662 -0.5827 0.0513 Uij ? ?
H(23) 0.0322 0.1916 -0.3175 0.0538 Uij ? ?
H(24) 0.2516 0.0722 -0.3993 0.0589 Uij ? ?
H(25) 0.1331 0.0112 -0.1303 0.0737 Uij ? ?
H(26) 0.2388 0.0007 -0.2279 0.0737 Uij ? ?
H(27) 0.3400 0.0188 0.0185 0.0770 Uij ? ?
H(28) 0.2711 -0.0286 0.0685 0.0770 Uij ? ?
H(29) 0.0883 -0.0018 0.1939 0.0784 Uij ? ?
H(30) 0.1224 0.0104 0.3852 0.0784 Uij ? ?
H(31) 0.0173 0.1123 0.3546 0.0696 Uij ? ?
H(32) -0.0526 0.0613 0.3441 0.0696 Uij ? ?
H(33) 0.1321 0.4611 -0.1170 0.0770 Uij ? ?
H(34) 0.0808 0.4288 -0.2723 0.0770 Uij ? ?
H(35) 0.0083 0.4616 -0.1305 0.0770 Uij ? ?
H(36) 0.4397 0.1320 0.0828 0.0805 Uij ? ?
H(37) 0.4185 0.1220 -0.1139 0.0805 Uij ? ?
H(38) 0.5365 0.1153 -0.0342 0.0805 Uij ? ?
H(39) -0.1731 0.3284 -0.3386 0.0853 Uij ? ?
H(40) -0.1359 0.2612 -0.4065 0.0853 Uij ? ?
H(41) -0.0960 0.2801 -0.2233 0.0853 Uij ? ?
H(42) 0.5192 0.1425 -0.5407 0.0861 Uij ? ?
H(43) 0.4406 0.1943 -0.6426 0.0861 Uij ? ?
H(44) 0.4739 0.2048 -0.4499 0.0861 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 56 0.018 0.009 'International Tables'
H 0 80 0.000 0.000 'International Tables'
N 0 8 0.031 0.018 'International Tables'
O 0 24 0.049 0.032 'International Tables'
Cl 0 4 0.364 0.702 'International Tables'
S 0 8 0.333 0.557 'International Tables'
Cu 0 4 -1.965 0.589 'International Tables'
