#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:14:47 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179745 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/41/7004104.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_7004104
loop_
_publ_author_name
'Kolotilov, Sergey V.'
'Schollmeyer, Dieter'
'Thompson, Laurence K.'
'Golub, Vladimir'
'Addison, Anthony W.'
'Pavlishchuk, Vitaly V.'
_publ_section_title
;
 Synthesis, structure and magnetic properties of oligometallic systems
 derived from di- and trinuclear copper(ii) amido-oximate complexes
;
_journal_issue                   22
_journal_name_full               'Dalton Transactions'
_journal_page_first              3007
_journal_page_last               3014
_journal_paper_doi               10.1039/b802822b
_journal_year                    2008
_chemical_formula_sum            'C13 H14 Cu2 N9 O10.25'
_chemical_formula_weight         611.86
_chemical_name_systematic
;
?
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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(5)
_cell_angle_gamma                120.000(5)
_cell_formula_units_Z            18
_cell_length_a                   26.551(5)
_cell_length_b                   26.551(5)
_cell_length_c                   19.976(5)
_cell_measurement_temperature    293(2)
_cell_volume                     12196(4)
_computing_cell_refinement       'Enraf Nonius Software V5'
_computing_data_collection       'Enraf Nonius Software V5'
_computing_data_reduction        'Corinc (Dräger, 1971)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CAD4 Enraf Nonius'
_diffrn_measurement_method       θ/2ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.1518
_diffrn_reflns_av_sigmaI/netI    0.1016
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            47903
_diffrn_reflns_theta_full        28.34
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    1.635
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5530
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.524
_refine_diff_density_min         -1.413
_refine_diff_density_rms         0.191
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         6759
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.1628
_refine_ls_R_factor_gt           0.0777
_refine_ls_shift/su_max          0.056
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1398P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2023
_refine_ls_wR_factor_ref         0.2488
_reflns_number_gt                3519
_reflns_number_total             6759
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b802822b.txt
_cod_data_source_block           publication_text
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal' according
to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               7004104
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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
C1 C 0.2271(4) -0.1179(3) 0.5725(4) 0.0566(19) Uani 1 1 d . . .
C2 C 0.2798(3) -0.1183(4) 0.5752(3) 0.061(2) Uani 1 1 d . . .
C3 C 0.2832(3) -0.1702(4) 0.5656(4) 0.056(2) Uani 1 1 d . . .
C4 C 0.3419(4) -0.2150(4) 0.5641(5) 0.075(3) Uani 1 1 d . . .
H32A H 0.3490 -0.2182 0.5171 0.090 Uiso 1 1 calc R . .
H32B H 0.3063 -0.2499 0.5770 0.090 Uiso 1 1 calc R . .
C5 C 0.3903(4) -0.2097(4) 0.6039(5) 0.077(3) Uani 1 1 d . . .
H29A H 0.3883 -0.2472 0.6041 0.093 Uiso 1 1 calc R . .
H29B H 0.3848 -0.2012 0.6497 0.093 Uiso 1 1 calc R . .
C6 C 0.4519(3) -0.1635(3) 0.5819(4) 0.059(2) Uani 1 1 d . . .
H26A H 0.4804 -0.1658 0.6102 0.071 Uiso 1 1 calc R . .
H26B H 0.4585 -0.1711 0.5361 0.071 Uiso 1 1 calc R . .
C7 C 0.5131(3) -0.0612(3) 0.5830(3) 0.0373(14) Uani 1 1 d . . .
C8 C 0.5182(3) -0.0029(3) 0.5872(3) 0.0357(14) Uani 1 1 d . . .
C9 C 0.5746(3) 0.0483(3) 0.5848(4) 0.0532(18) Uani 1 1 d . . .
C10 C 0.3671(4) 0.1171(3) 0.5442(3) 0.0524(19) Uani 1 1 d . . .
H17A H 0.3342 0.0833 0.5244 0.063 Uiso 1 1 calc R . .
H17B H 0.3758 0.1509 0.5172 0.063 Uiso 1 1 calc R . .
C11 C 0.3527(3) 0.1257(3) 0.6150(3) 0.0512(18) Uani 1 1 d . . .
H15A H 0.3834 0.1622 0.6328 0.061 Uiso 1 1 calc R . .
H15B H 0.3166 0.1264 0.6158 0.061 Uiso 1 1 calc R . .
C12 C 0.3511(3) 0.0852(3) 0.7295(3) 0.0481(17) Uani 1 1 d . . .
H19A H 0.3824 0.1238 0.7408 0.058 Uiso 1 1 calc R . .
H19B H 0.3150 0.0807 0.7470 0.058 Uiso 1 1 calc R . .
C13 C 0.3627(3) 0.0400(3) 0.7585(3) 0.0494(17) Uani 1 1 d . . .
H27A H 0.3291 0.0017 0.7519 0.059 Uiso 1 1 calc R . .
H27B H 0.3698 0.0464 0.8062 0.059 Uiso 1 1 calc R . .
N1 N 0.3316(3) -0.0711(3) 0.5865(3) 0.0619(18) Uani 1 1 d . . .
N2 N 0.3353(2) -0.1649(3) 0.5743(3) 0.0654(19) Uani 1 1 d . . .
N3 N 0.4595(2) -0.1047(2) 0.5862(3) 0.0457(13) Uani 1 1 d . . .
N4 N 0.4706(2) -0.0011(2) 0.5935(3) 0.0425(13) Uani 1 1 d . . .
N5 N 0.1837(4) -0.1188(3) 0.5686(4) 0.076(2) Uani 1 1 d . . .
N6 N 0.6191(4) 0.0876(3) 0.5831(5) 0.090(3) Uani 1 1 d . . .
N7 N 0.4187(2) 0.1087(2) 0.5467(3) 0.0424(13) Uani 1 1 d . . .
N8 N 0.3472(2) 0.0767(2) 0.6555(3) 0.0413(12) Uani 1 1 d . . .
N9 N 0.4146(3) 0.0436(3) 0.7247(3) 0.0480(14) Uani 1 1 d . . .
O1 O 0.3309(3) -0.0250(2) 0.5936(2) 0.0662(16) Uani 1 1 d . . .
O2 O 0.2372(2) -0.2157(3) 0.5493(3) 0.0677(16) Uani 1 1 d . . .
O3 O 0.55953(17) -0.06301(18) 0.5769(2) 0.0392(10) Uani 1 1 d . . .
O4 O 0.4750(2) 0.0504(2) 0.5974(3) 0.0568(13) Uani 1 1 d . . .
O5 O 0.39652(18) -0.07461(19) 0.7099(2) 0.0409(10) Uani 1 1 d . . .
O6 O 0.2212(8) 0.0163(7) 0.5881(10) 0.125(6) Uani 0.50 1 d P . .
O7 O 0.2081(8) 0.0587(8) 0.6910(13) 0.157(9) Uani 0.50 1 d P . .
O8 O 0.2357(3) -0.2780(4) 0.4409(4) 0.137(4) Uani 1 1 d . . .
O9 O 0.1802(11) -0.3908(12) 0.3632(19) 0.211(13) Uani 0.50 1 d P . .
O10 O 0.308(3) -0.344(6) 0.4370(19) 0.36(3) Uiso 0.50 1 d P . .
O11 O 0.208(3) 0.069(3) 0.520(3) 0.42(3) Uiso 0.50 1 d P . .
O12 O 0.207(3) -0.488(4) 0.344(4) 0.52(5) Uiso 0.50 1 d P . .
O13 O 0.184(2) -0.365(2) 0.306(3) 0.32(2) Uiso 0.50 1 d P . .
O14 O 0.1790(15) 0.0231(15) 0.4523(19) 0.245(13) Uiso 0.50 1 d P . .
O15 O 0.195(4) -0.407(4) 0.298(5) 0.30(4) Uiso 0.25 1 d P . .
Cu1 Cu 0.39875(3) -0.08442(4) 0.59433(4) 0.0440(3) Uani 1 1 d . . .
Cu2 Cu 0.40980(3) 0.05959(3) 0.62698(4) 0.0388(3) Uani 1 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'
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
_geom_angle_publ_flag
N5 C1 C2 177.8(9) . . ?
N1 C2 C1 124.1(9) . . ?
N1 C2 C3 113.2(7) . . ?
C1 C2 C3 122.7(7) . . ?
O2 C3 N2 126.5(8) . . ?
O2 C3 C2 117.3(7) . . ?
N2 C3 C2 116.2(7) . . ?
N2 C4 C5 110.0(7) . . ?
C4 C5 C6 117.1(8) . . ?
N3 C6 C5 110.8(6) . . ?
O3 C7 N3 128.4(6) . . ?
O3 C7 C8 117.5(6) . . ?
N3 C7 C8 114.0(5) . . ?
N4 C8 C9 123.0(6) . . ?
N4 C8 C7 117.4(6) . . ?
C9 C8 C7 119.6(5) . . ?
N6 C9 C8 178.5(8) . . ?
N7 C10 C11 108.1(5) . . ?
N8 C11 C10 107.6(5) . . ?
C13 C12 N8 106.8(5) . . ?
C12 C13 N9 109.1(5) . . ?
O1 N1 C2 115.4(7) . . ?
O1 N1 Cu1 128.5(6) . . ?
C2 N1 Cu1 116.0(6) . . ?
C3 N2 C4 118.9(7) . . ?
C3 N2 Cu1 114.6(6) . . ?
C4 N2 Cu1 126.3(5) . . ?
C7 N3 C6 116.3(5) . . ?
C7 N3 Cu1 116.5(4) . . ?
C6 N3 Cu1 127.2(4) . . ?
C8 N4 O4 117.5(6) . . ?
C8 N4 Cu1 110.9(4) . . ?
O4 N4 Cu1 131.6(4) . . ?
C10 N7 Cu2 107.8(4) . . ?
C11 N8 C12 116.2(5) . . ?
C11 N8 Cu2 108.3(4) . . ?
C12 N8 Cu2 108.2(4) . . ?
C13 N9 Cu2 107.3(4) . . ?
N1 O1 Cu2 123.2(5) . . ?
N4 O4 Cu2 121.5(4) . . ?
O10 O10 O10 60.00(4) 3_655 2_545 ?
O10 O10 O12 145(8) 3_655 . ?
O10 O10 O12 97(10) 2_545 . ?
N3 Cu1 N2 93.5(3) . . ?
N3 Cu1 N1 169.5(3) . . ?
N2 Cu1 N1 79.8(3) . . ?
N3 Cu1 N4 81.2(2) . . ?
N2 Cu1 N4 167.2(2) . . ?
N1 Cu1 N4 103.7(3) . . ?
N3 Cu1 O5 100.6(2) . . ?
N2 Cu1 O5 105.3(2) . . ?
N1 Cu1 O5 89.0(2) . . ?
N4 Cu1 O5 87.14(18) . . ?
O4 Cu2 N7 90.9(2) . . ?
O4 Cu2 N8 174.8(2) . . ?
N7 Cu2 N8 85.5(2) . . ?
O4 Cu2 N9 96.5(2) . . ?
N7 Cu2 N9 155.9(2) . . ?
N8 Cu2 N9 85.4(2) . . ?
O4 Cu2 O1 102.9(2) . . ?
N7 Cu2 O1 99.1(2) . . ?
N8 Cu2 O1 81.3(2) . . ?
N9 Cu2 O1 101.5(2) . . ?
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
C1 N5 1.144(10) . ?
C1 C2 1.405(12) . ?
C2 N1 1.337(9) . ?
C2 C3 1.438(12) . ?
C3 O2 1.257(9) . ?
C3 N2 1.330(10) . ?
C4 N2 1.439(11) . ?
C4 C5 1.459(12) . ?
C5 C6 1.539(11) . ?
C6 N3 1.474(9) . ?
C7 O3 1.263(7) . ?
C7 N3 1.311(8) . ?
C7 C8 1.488(8) . ?
C8 N4 1.295(8) . ?
C8 C9 1.434(10) . ?
C9 N6 1.119(10) . ?
C10 N7 1.495(9) . ?
C10 C11 1.511(9) . ?
C11 N8 1.475(8) . ?
C12 C13 1.494(9) . ?
C12 N8 1.492(8) . ?
C13 N9 1.494(9) . ?
N1 O1 1.239(8) . ?
N1 Cu1 1.991(6) . ?
N2 Cu1 1.990(7) . ?
N3 Cu1 1.946(5) . ?
N4 O4 1.316(7) . ?
N4 Cu1 2.076(6) . ?
N7 Cu2 2.006(5) . ?
N8 Cu2 2.012(5) . ?
N9 Cu2 2.016(5) . ?
O1 Cu2 2.274(6) . ?
O4 Cu2 1.956(4) . ?
O5 Cu1 2.327(4) . ?
O10 O10 1.02(11) 3_655 ?
O10 O10 1.02(11) 2_545 ?
O10 O12 3.87(13) . ?
