#------------------------------------------------------------------------------
#$Date: 2016-03-25 15:44:27 +0100 (vie 25 de mar de 2016) $
#$Revision: 179987 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/81/7028191.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_7028191
loop_
_publ_author_name
'Bernhardt, Paul V.'
'Hayes, Elizabeth J.'
_publ_section_title
;
 Copper(II) complexes of mono- and di-nucleating
 hexaamines †
;
_journal_issue                   6
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1037
_journal_paper_doi               10.1039/a707209k
_journal_year                    1998
_chemical_formula_sum            'C18 H51 Cl3 Cu2 N6 O16'
_chemical_formula_weight         841.08
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 107.58(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.738(9)
_cell_length_b                   8.391(3)
_cell_length_c                   16.348(8)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      10
_cell_volume                     3366(2)
_computing_cell_refinement       CAD4
_computing_data_collection       CAD4
_computing_data_reduction        XTAL
_computing_molecular_graphics    PLATON
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD4'
_diffrn_measurement_method       'omega-2theta scans'
_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  0.0753
_diffrn_reflns_av_sigmaI/netI    0.0419
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            2964
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         1.66
_diffrn_standards_interval_count 250
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.577
_exptl_absorpt_correction_T_max  1.20
_exptl_absorpt_correction_T_min  1.00
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.660
_exptl_crystal_description       prism
_exptl_crystal_F_000             1752
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.529
_refine_diff_density_min         -1.409
_refine_diff_density_rms         0.380
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.120
_refine_ls_goodness_of_fit_obs   1.168
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         2962
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.120
_refine_ls_restrained_S_obs      1.168
_refine_ls_R_factor_all          0.1293
_refine_ls_R_factor_obs          0.0948
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1842P)²+5.0446P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2706
_refine_ls_wR_factor_obs         0.2378
_reflns_number_observed          2144
_reflns_number_total             2962
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            k707209sup1.cif
_cod_data_source_block           cuompeh
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1842P)^2^+5.0446P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1842P)^2^+5.0446P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3365.7(24)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7028191
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Cu1 Cu 0.11832(3) 0.11141(10) 0.00254(6) 0.0530(4) Uani 1 d . .
O1A O 0.0594(3) -0.0199(9) 0.0595(5) 0.021(2) Uiso 0.50 d P 1
H11 H 0.0456(3) 0.0358(9) 0.0886(5) 0.032 Uiso 0.50 d PR 1
H12 H 0.0694(3) -0.0790(9) 0.0593(5) 0.032 Uiso 1 d R 1
O1B O 0.0579(3) -0.0373(10) 0.0255(7) 0.035(2) Uiso 0.50 d P 2
N1 N 0.1717(2) 0.2498(6) -0.0359(3) 0.0404(12) Uani 1 d . .
N2 N 0.1109(3) 0.3017(9) 0.0763(4) 0.063(2) Uani 1 d . .
N3 N 0.1131(3) -0.0204(7) -0.1056(5) 0.060(2) Uani 1 d . .
C1 C 0.2287(3) 0.2039(8) 0.0123(5) 0.045(2) Uani 1 d . .
H1A H 0.2336(3) 0.0912(8) 0.0039(5) 0.054 Uiso 1 d R .
H1B H 0.2341(3) 0.2209(8) 0.0730(5) 0.054 Uiso 1 d R .
C2 C 0.1589(3) 0.4175(7) -0.0165(5) 0.049(2) Uani 1 d . .
H2A H 0.1883(3) 0.4885(7) -0.0181(5) 0.059 Uiso 1 d R .
H2B H 0.1257(3) 0.4534(7) -0.0587(5) 0.059 Uiso 1 d R .
C3 C 0.1522(4) 0.4218(10) 0.0681(6) 0.066(2) Uani 1 d . .
H3A H 0.1410(4) 0.5276(10) 0.0800(6) 0.079 Uiso 1 d R .
H3B H 0.1868(4) 0.3983(10) 0.1104(6) 0.079 Uiso 1 d R .
C4 C 0.1586(3) 0.2172(9) -0.1289(5) 0.056(2) Uani 1 d . .
H4A H 0.1873(3) 0.2586(9) -0.1500(5) 0.067 Uiso 1 d R .
H4B H 0.1248(3) 0.2702(9) -0.1594(5) 0.067 Uiso 1 d R .
C5 C 0.1528(4) 0.0424(11) -0.1432(6) 0.067(2) Uani 1 d . .
H5A H 0.1410(4) 0.0210(11) -0.2044(6) 0.080 Uiso 1 d R .
H5B H 0.1877(4) -0.0092(11) -0.1182(6) 0.080 Uiso 1 d R .
C6 C 0.1199(5) 0.2649(16) 0.1677(6) 0.092(3) Uani 1 d . .
H6A H 0.0932(5) 0.1881(16) 0.1722(6) 0.138 Uiso 1 d R .
H6B H 0.1162(5) 0.3600(16) 0.1981(6) 0.138 Uiso 1 d R .
H6C H 0.1558(5) 0.2215(16) 0.1922(6) 0.138 Uiso 1 d R .
C7 C 0.0554(4) 0.3693(13) 0.0385(8) 0.082(3) Uani 1 d . .
H7A H 0.0287(4) 0.2929(13) 0.0432(8) 0.123 Uiso 1 d R .
H7B H 0.0502(4) 0.3926(13) -0.0209(8) 0.123 Uiso 1 d R .
H7C H 0.0515(4) 0.4653(13) 0.0679(8) 0.123 Uiso 1 d R .
C8 C 0.0571(3) -0.0009(11) -0.1639(6) 0.074(2) Uani 1 d . .
H8A H 0.0315(3) -0.0431(11) -0.1373(6) 0.110 Uiso 1 d R .
H8B H 0.0536(3) -0.0571(11) -0.2164(6) 0.110 Uiso 1 d R .
H8C H 0.0497(3) 0.1102(11) -0.1761(6) 0.110 Uiso 1 d R .
C9 C 0.1229(4) -0.1979(9) -0.0889(8) 0.092(3) Uani 1 d . .
H9A H 0.0967(4) -0.2396(9) -0.0633(8) 0.139 Uiso 1 d R .
H9B H 0.1590(4) -0.2157(9) -0.0512(8) 0.139 Uiso 1 d R .
H9C H 0.1188(4) -0.2506(9) -0.1426(8) 0.139 Uiso 1 d R .
Cl1 Cl 0.22939(11) -0.1412(2) 0.15393(14) 0.0696(7) Uani 1 d . .
O11 O 0.1838(4) -0.0438(11) 0.1092(6) 0.119(3) Uani 1 d . .
O12A O 0.2715(12) -0.0410(36) 0.1949(21) 0.135(10) Uiso 0.46(3) d P 3
O13A O 0.2152(10) -0.2256(28) 0.2154(14) 0.103(8) Uiso 0.46(3) d P 3
O14A O 0.2393(9) -0.2414(28) 0.0869(15) 0.098(7) Uiso 0.46(3) d P 3
O12B O 0.2394(10) -0.1541(27) 0.2453(14) 0.120(8) Uiso 0.54(3) d P 4
O13B O 0.2827(5) -0.0634(16) 0.1598(10) 0.072(5) Uiso 0.54(3) d P 4
O14B O 0.2318(9) -0.2915(30) 0.1140(14) 0.120(7) Uiso 0.54(3) d P 4
Cl2 Cl 0.0000 0.4825(3) 0.7500 0.0522(7) Uani 1 d S .
O21 O 0.0000 0.6458(18) 0.7500 0.225(12) Uani 1 d S .
O22A O -0.0470(18) 0.4318(58) 0.6954(27) 0.105(14) Uiso 0.25(3) d P 3
O23A O 0.0174(15) 0.4063(40) 0.8332(19) 0.072(10) Uiso 0.25(3) d P 3
O24A O 0.0502(15) 0.4303(43) 0.7387(24) 0.083(11) Uiso 0.25(3) d P 3
O22B O -0.0278(18) 0.4967(72) 0.6675(29) 0.117(15) Uiso 0.25(3) d P 4
O23B O 0.0605(17) 0.4849(54) 0.7729(28) 0.095(12) Uiso 0.25(3) d P 4
O24B O -0.0170(15) 0.3843(34) 0.8092(20) 0.077(12) Uiso 0.25(3) d P 4
O3 O 0.0903(7) -0.2203(21) 0.1554(10) 0.202(6) Uani 1 d . .
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'
Cl Cl 0.1484 0.1585 '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'
O O 0.0106 0.0060 '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
N1 Cu1 N2 85.9(3) . .
N1 Cu1 N3 85.2(2) . .
N2 Cu1 N3 159.1(3) . .
N1 Cu1 O1B 172.6(3) . .
N2 Cu1 O1B 98.7(3) . .
N3 Cu1 O1B 88.6(3) . .
N1 Cu1 O1A 172.5(3) . .
N2 Cu1 O1A 86.8(3) . .
N3 Cu1 O1A 102.3(3) . .
N1 Cu1 O11 98.1(2) . .
N2 Cu1 O11 99.5(3) . .
N3 Cu1 O11 100.4(3) . .
O1B Cu1 O11 86.8(3) . .
O1A Cu1 O11 81.4(3) . .
C4 N1 C1 112.2(5) . .
C4 N1 C2 113.2(5) . .
C1 N1 C2 112.0(5) . .
C4 N1 Cu1 104.2(4) . .
C1 N1 Cu1 109.7(4) . .
C2 N1 Cu1 104.9(4) . .
C6 N2 C7 109.8(7) . .
C6 N2 C3 109.4(7) . .
C7 N2 C3 108.9(7) . .
C6 N2 Cu1 114.8(7) . .
C7 N2 Cu1 107.6(6) . .
C3 N2 Cu1 106.1(5) . .
C5 N3 C8 111.4(7) . .
C5 N3 C9 109.6(7) . .
C8 N3 C9 107.4(6) . .
C5 N3 Cu1 107.5(5) . .
C8 N3 Cu1 107.0(5) . .
C9 N3 Cu1 114.1(6) . .
N1 C1 C1 114.2(7) . 7
C3 C2 N1 108.9(6) . .
C2 C3 N2 111.2(7) . .
N1 C4 C5 109.0(6) . .
N3 C5 C4 110.1(7) . .
O13A Cl1 O12A 107.7(15) . .
O13A Cl1 O11 108.2(9) . .
O12A Cl1 O11 107.6(13) . .
O14B Cl1 O11 114.3(10) . .
O14B Cl1 O12B 112.9(12) . .
O11 Cl1 O12B 115.7(9) . .
O13A Cl1 O14A 113.5(13) . .
O12A Cl1 O14A 115.2(16) . .
O11 Cl1 O14A 104.3(10) . .
O14B Cl1 O13B 104.4(11) . .
O11 Cl1 O13B 112.1(6) . .
O12B Cl1 O13B 95.3(11) . .
Cl1 O11 Cu1 164.2(6) . .
O22B Cl2 O22B 169.8(52) . 2_556
O22A Cl2 O22A 142.9(42) . 2_556
O22B Cl2 O21 84.9(26) . .
O22B Cl2 O21 84.9(26) 2_556 .
O22A Cl2 O21 108.6(21) . .
O22A Cl2 O21 108.6(21) 2_556 .
O22A Cl2 O24A 119.2(24) . .
O22A Cl2 O24A 46.9(21) 2_556 .
O21 Cl2 O24A 107.9(15) . .
O22A Cl2 O24A 46.9(21) . 2_556
O22A Cl2 O24A 119.2(24) 2_556 2_556
O21 Cl2 O24A 107.9(15) . 2_556
O24A Cl2 O24A 144.3(30) . 2_556
O22B Cl2 O24B 123.8(26) . .
O22B Cl2 O24B 63.0(26) 2_556 .
O21 Cl2 O24B 125.0(11) . .
O22B Cl2 O24B 63.0(26) . 2_556
O22B Cl2 O24B 123.8(26) 2_556 2_556
O21 Cl2 O24B 125.0(11) . 2_556
O24B Cl2 O24B 109.9(22) . 2_556
O22A Cl2 O23A 43.2(22) . 2_556
O22A Cl2 O23A 116.5(22) 2_556 2_556
O21 Cl2 O23A 116.3(13) . 2_556
O24A Cl2 O23A 77.1(19) . 2_556
O24A Cl2 O23A 87.2(18) 2_556 2_556
O22A Cl2 O23A 116.5(22) . .
O22A Cl2 O23A 43.2(22) 2_556 .
O21 Cl2 O23A 116.3(13) . .
O24A Cl2 O23A 87.2(18) . .
O24A Cl2 O23A 77.1(19) 2_556 .
O23A Cl2 O23A 127.5(26) 2_556 .
O22B Cl2 O23B 62.7(25) . 2_556
O22B Cl2 O23B 117.1(25) 2_556 2_556
O21 Cl2 O23B 89.2(17) . 2_556
O24B Cl2 O23B 70.7(19) . 2_556
O24B Cl2 O23B 110.3(21) 2_556 2_556
O23A O22A O24A 136.4(51) 2_556 2_556
O23A O22A Cl2 74.0(32) 2_556 .
O24A O22A Cl2 70.9(28) 2_556 .
O22A O23A Cl2 62.8(27) 2_556 .
O22A O23A O24A 112.6(32) 2_556 2_556
Cl2 O23A O24A 51.0(14) . 2_556
O22A O24A Cl2 62.2(26) 2_556 .
O22A O24A O23A 107.3(33) 2_556 2_556
Cl2 O24A O23A 51.9(14) . 2_556
Cl2 O22B O24B 62.2(24) . 2_556
Cl2 O22B O23B 64.0(23) . 2_556
O24B O22B O23B 110.5(37) 2_556 2_556
O22B O23B Cl2 53.3(21) 2_556 .
O22B O23B O24B 100.6(29) 2_556 2_556
Cl2 O23B O24B 53.3(17) . 2_556
Cl2 O24B O22B 54.8(20) . 2_556
Cl2 O24B O23B 56.1(15) . 2_556
O22B O24B O23B 99.6(28) 2_556 2_556
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N1 2.037(5) .
Cu1 N2 2.044(7) .
Cu1 N3 2.056(7) .
Cu1 O1B 2.114(9) .
Cu1 O1A 2.287(7) .
Cu1 O11 2.408(8) .
N1 C4 1.480(9) .
N1 C1 1.490(8) .
N1 C2 1.501(8) .
N2 C6 1.474(11) .
N2 C7 1.485(11) .
N2 C3 1.500(12) .
N3 C5 1.441(11) .
N3 C8 1.479(10) .
N3 C9 1.521(10) .
C1 C1 1.494(13) 7
C2 C3 1.443(11) .
C4 C5 1.486(12) .
Cl1 O13A 1.37(2) .
Cl1 O12A 1.38(3) .
Cl1 O14B 1.43(2) .
Cl1 O11 1.436(8) .
Cl1 O12B 1.44(2) .
Cl1 O14A 1.46(2) .
Cl1 O13B 1.496(14) .
Cl2 O22B 1.33(5) .
Cl2 O22B 1.33(5) 2_556
Cl2 O22A 1.34(4) .
Cl2 O22A 1.34(4) 2_556
Cl2 O21 1.37(2) .
Cl2 O24A 1.43(3) .
Cl2 O24A 1.43(3) 2_556
Cl2 O24B 1.44(3) .
Cl2 O24B 1.44(3) 2_556
Cl2 O23A 1.45(3) 2_556
Cl2 O23A 1.45(3) .
Cl2 O23B 1.49(4) 2_556
O22A O23A 1.03(5) 2_556
O22A O24A 1.11(5) 2_556
O23A O22A 1.03(5) 2_556
O23A O24A 1.79(5) 2_556
O24A O22A 1.11(5) 2_556
O24A O23A 1.79(5) 2_556
O22B O24B 1.45(7) 2_556
O22B O23B 1.47(6) 2_556
O23B O22B 1.47(6) 2_556
O23B O24B 1.69(5) 2_556
O24B O22B 1.45(7) 2_556
O24B O23B 1.69(5) 2_556
