#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:10:25 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179955 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/50/7025020.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_7025020
loop_
_publ_author_name
'Maxim, Catalin'
'Sorace, Lorenzo'
'Khuntia, Panchanana'
'Madalan, Augustin M.'
'Kravtsov, Victor'
'Lascialfari, Alessandro'
'Caneschi, Andrea'
'Journaux, Yves'
'Andruh, Marius'
_publ_section_title
;
 A missing high-spin molecule in the family of cyanido-bridged
 heptanuclear heterometal complexes, [(LCuII)6FeIII(CN)6]3+, and its CoIII
 and CrIII analogues, accompanied in the crystal by a novel octameric
 water cluster
;
_journal_issue                   20
_journal_name_full               'Dalton Transactions'
_journal_page_first              4838
_journal_paper_doi               10.1039/b924505g
_journal_volume                  39
_journal_year                    2010
_chemical_formula_sum            'C22 H40 Cl2 Cu2 N4 O15'
_chemical_formula_weight         798.56
_chemical_name_systematic
;
?
;
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 90.000(4)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            8
_cell_length_a                   17.5460(11)
_cell_length_b                   37.8030(11)
_cell_length_c                   9.994(2)
_cell_measurement_reflns_used    584
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.5
_cell_volume                     6628.9(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'phi and omega 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  0.0675
_diffrn_reflns_av_sigmaI/netI    0.0666
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            10387
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         2.41
_exptl_absorpt_coefficient_mu    1.516
_exptl_absorpt_correction_T_max  0.8632
_exptl_absorpt_correction_T_min  0.7514
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.600
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3296
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.558
_refine_diff_density_min         -0.614
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.008(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     234
_refine_ls_number_reflns         3249
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0440
_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)+(0.0563P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1002
_refine_ls_wR_factor_ref         0.1055
_reflns_number_gt                2458
_reflns_number_total             3249
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b924505g.txt
_cod_data_source_block           cmmn1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' 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_cell_volume        6628.9(15)
_cod_original_sg_symbol_H-M      Fdd2
_cod_database_code               7025020
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x+1/4, y+1/4, z+1/4'
'x+1/4, -y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'-x+1/4, y+3/4, z+3/4'
'x+1/4, -y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'-x+3/4, y+1/4, z+3/4'
'x+3/4, -y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'-x+3/4, y+3/4, z+1/4'
'x+3/4, -y+3/4, z+1/4'
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 0.10655(3) -0.020999(15) 0.59654(5) 0.03607(17) Uani 1 1 d . . .
O1 O 0.10497(17) 0.02247(8) 0.5003(3) 0.0362(8) Uani 1 1 d . . .
O1W O 0.0393(2) -0.04174(9) 0.4602(4) 0.0419(9) Uani 1 1 d D . .
H1W1 H 0.060(2) -0.0372(14) 0.380(2) 0.063 Uiso 1 1 d D . .
H2W1 H -0.0055(15) -0.0320(16) 0.460(5) 0.063 Uiso 1 1 d D . .
O2W O 0.0000 0.0000 0.7383(5) 0.0513(14) Uani 1 2 d SD . .
H1W2 H 0.020(3) 0.0158(9) 0.801(2) 0.077 Uiso 1 1 d D . .
N1 N 0.1849(2) -0.00493(12) 0.7188(4) 0.0407(10) Uani 1 1 d . . .
N2 N 0.1184(3) -0.06849(12) 0.6907(5) 0.0508(12) Uani 1 1 d . . .
C1 C 0.1454(2) 0.05179(12) 0.5275(5) 0.0343(10) Uani 1 1 d . . .
C2 C 0.1357(3) 0.08103(13) 0.4420(6) 0.0401(12) Uani 1 1 d . . .
H2 H 0.1026 0.0790 0.3672 0.048 Uiso 1 1 calc R . .
C3 C 0.1728(3) 0.11232(15) 0.4643(6) 0.0516(14) Uani 1 1 d . . .
H3 H 0.1657 0.1317 0.4050 0.062 Uiso 1 1 calc R . .
C4 C 0.2214(3) 0.11573(16) 0.5752(8) 0.0681(19) Uani 1 1 d . . .
H4 H 0.2453 0.1378 0.5936 0.082 Uiso 1 1 calc R . .
C5 C 0.2341(3) 0.08798(18) 0.6546(6) 0.0562(15) Uani 1 1 d . . .
H5 H 0.2687 0.0903 0.7272 0.067 Uiso 1 1 calc R . .
C6 C 0.1971(3) 0.05483(14) 0.6333(5) 0.0395(12) Uani 1 1 d . . .
C7 C 0.2135(3) 0.02581(16) 0.7238(5) 0.0482(14) Uani 1 1 d . . .
H7 H 0.2491 0.0303 0.7934 0.058 Uiso 1 1 calc R . .
C8 C 0.2111(3) -0.03190(17) 0.8139(6) 0.0605(16) Uani 1 1 d . . .
H8A H 0.2211 -0.0211 0.9024 0.073 Uiso 1 1 calc R . .
H8B H 0.2588 -0.0430 0.7815 0.073 Uiso 1 1 calc R . .
C9 C 0.1478(3) -0.05975(17) 0.8251(6) 0.0634(18) Uani 1 1 d . . .
H9A H 0.1682 -0.0814 0.8682 0.076 Uiso 1 1 calc R . .
H9B H 0.1059 -0.0505 0.8814 0.076 Uiso 1 1 calc R . .
C10 C 0.1742(3) -0.08924(15) 0.6117(7) 0.0686(19) Uani 1 1 d . . .
H10A H 0.1855 -0.1114 0.6585 0.103 Uiso 1 1 calc R . .
H10B H 0.2212 -0.0755 0.6012 0.103 Uiso 1 1 calc R . .
H10C H 0.1527 -0.0945 0.5234 0.103 Uiso 1 1 calc R . .
C11 C 0.0457(3) -0.08943(16) 0.7011(7) 0.0688(19) Uani 1 1 d . . .
H11A H 0.0271 -0.0951 0.6112 0.103 Uiso 1 1 calc R . .
H11B H 0.0073 -0.0754 0.7486 0.103 Uiso 1 1 calc R . .
H11C H 0.0554 -0.1114 0.7504 0.103 Uiso 1 1 calc R . .
Cl1A Cl 0.09460(8) 0.05434(4) 0.03219(13) 0.0461(3) Uani 0.740(6) 1 d PD A 1
O1CL O 0.1352(8) 0.0363(3) 0.1275(12) 0.165(5) Uani 0.740(6) 1 d PD A 1
O2CL O 0.0535(7) 0.0266(3) -0.0285(9) 0.161(5) Uani 0.740(6) 1 d PD A 1
O3CL O 0.0346(6) 0.0743(3) 0.0820(11) 0.200(6) Uani 0.740(6) 1 d PD A 1
O4CL O 0.1335(6) 0.0727(2) -0.0686(11) 0.131(4) Uani 0.740(6) 1 d PD A 1
Cl1B Cl 0.09460(8) 0.05434(4) 0.03219(13) 0.0461(3) Uani 0.260(6) 1 d PD A 2
O5CL O 0.1492(10) 0.0276(5) 0.054(2) 0.069 Uiso 0.260(6) 1 d PD A 2
O6CL O 0.1300(9) 0.0860(3) 0.0762(17) 0.069 Uiso 0.260(6) 1 d PD A 2
O7CL O 0.0817(11) 0.0574(5) -0.1006(12) 0.069 Uiso 0.260(6) 1 d PD A 2
O8CL O 0.0396(8) 0.0498(5) 0.1302(15) 0.069 Uiso 0.260(6) 1 d PD A 2
O1WS O 0.0919(2) 0.96606(13) 0.2096(4) 0.0612(11) Uani 1 1 d D . .
H1WS H 0.089(3) 0.9887(7) 0.179(7) 0.092 Uiso 1 1 d D . .
H2WS H 0.053(3) 0.9557(12) 0.161(6) 0.092 Uiso 1 1 d 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'
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'
Cl Cl 0.1484 0.1585 '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
O1 Cu1 N1 93.34(16) .
O1 Cu1 O1W 89.16(14) .
N1 Cu1 O1W 171.28(16) .
O1 Cu1 N2 174.29(16) .
N1 Cu1 N2 85.0(2) .
O1W Cu1 N2 91.72(18) .
O1 Cu1 O2W 90.08(12) .
N1 Cu1 O2W 94.27(14) .
O1W Cu1 O2W 94.08(13) .
N2 Cu1 O2W 95.48(14) .
C1 O1 Cu1 127.0(3) .
Cu1 O1W H1W1 108(3) .
Cu1 O1W H2W1 112(4) .
H1W1 O1W H2W1 106(3) .
Cu1 O2W Cu1 110.19(19) 2
Cu1 O2W H1W2 117(4) 2
Cu1 O2W H1W2 108(4) .
C7 N1 C8 119.2(5) .
C7 N1 Cu1 126.4(4) .
C8 N1 Cu1 114.4(4) .
C9 N2 C10 111.9(5) .
C9 N2 C11 110.5(5) .
C10 N2 C11 108.6(5) .
C9 N2 Cu1 105.0(4) .
C10 N2 Cu1 106.8(3) .
C11 N2 Cu1 114.1(4) .
O1 C1 C6 124.3(4) .
O1 C1 C2 117.5(4) .
C6 C1 C2 118.2(4) .
C3 C2 C1 121.5(5) .
C3 C2 H2 119.3 .
C1 C2 H2 119.3 .
C2 C3 C4 119.8(6) .
C2 C3 H3 120.1 .
C4 C3 H3 120.1 .
C5 C4 C3 119.9(5) .
C5 C4 H4 120.1 .
C3 C4 H4 120.1 .
C4 C5 C6 121.7(5) .
C4 C5 H5 119.1 .
C6 C5 H5 119.1 .
C1 C6 C5 118.7(5) .
C1 C6 C7 122.6(5) .
C5 C6 C7 118.7(5) .
N1 C7 C6 126.2(5) .
N1 C7 H7 116.9 .
C6 C7 H7 116.9 .
N1 C8 C9 107.3(5) .
N1 C8 H8A 110.3 .
C9 C8 H8A 110.3 .
N1 C8 H8B 110.3 .
C9 C8 H8B 110.3 .
H8A C8 H8B 108.5 .
N2 C9 C8 109.9(5) .
N2 C9 H9A 109.7 .
C8 C9 H9A 109.7 .
N2 C9 H9B 109.7 .
C8 C9 H9B 109.7 .
H9A C9 H9B 108.2 .
N2 C10 H10A 109.5 .
N2 C10 H10B 109.5 .
H10A C10 H10B 109.5 .
N2 C10 H10C 109.5 .
H10A C10 H10C 109.5 .
H10B C10 H10C 109.5 .
N2 C11 H11A 109.5 .
N2 C11 H11B 109.5 .
H11A C11 H11B 109.5 .
N2 C11 H11C 109.5 .
H11A C11 H11C 109.5 .
H11B C11 H11C 109.5 .
O1CL Cl1A O3CL 114.5(7) .
O1CL Cl1A O4CL 119.5(7) .
O3CL Cl1A O4CL 110.9(5) .
O1CL Cl1A O2CL 101.2(6) .
O3CL Cl1A O2CL 99.9(8) .
O4CL Cl1A O2CL 108.0(7) .
H1WS O1WS H2WS 100(3) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O1 1.904(3) .
Cu1 N1 1.937(4) .
Cu1 O1W 1.966(4) .
Cu1 N2 2.037(4) .
Cu1 O2W 2.477(3) .
O1 C1 1.344(5) .
O1W H1W1 0.891(12) .
O1W H2W1 0.87(3) .
O2W Cu1 2.477(3) 2
O2W H1W2 0.934(14) .
N1 C7 1.267(7) .
N1 C8 1.468(7) .
N2 C9 1.477(8) .
N2 C10 1.481(7) .
N2 C11 1.505(7) .
C1 C6 1.398(7) .
C1 C2 1.407(7) .
C2 C3 1.369(7) .
C2 H2 0.9500 .
C3 C4 1.404(8) .
C3 H3 0.9500 .
C4 C5 1.334(9) .
C4 H4 0.9500 .
C5 C6 1.428(8) .
C5 H5 0.9500 .
C6 C7 1.451(8) .
C7 H7 0.9500 .
C8 C9 1.535(9) .
C8 H8A 0.9900 .
C8 H8B 0.9900 .
C9 H9A 0.9900 .
C9 H9B 0.9900 .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
Cl1A O1CL 1.370(7) .
Cl1A O3CL 1.388(7) .
Cl1A O4CL 1.400(7) .
Cl1A O2CL 1.410(7) .
O1WS H1WS 0.910(19) .
O1WS H2WS 0.928(17) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1W1 O1WS 0.891(12) 1.802(14) 2.685(5) 171(5) 1_545
O1W H2W1 O1 0.87(3) 1.826(19) 2.664(5) 162(5) 2
O2W H1W2 O2CL 0.934(14) 1.847(17) 2.706(9) 152(2) 1_556
O1WS H1WS O1CL 0.910(19) 2.043(18) 2.883(12) 153(4) 1_565
O1WS H2WS O3CL 0.928(17) 2.065(16) 2.981(11) 169(5) 2_565
