#------------------------------------------------------------------------------
#$Date: 2018-09-10 12:34:14 +0300 (Mon, 10 Sep 2018) $
#$Revision: 210734 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/11/36/7113607.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_7113607
loop_
_publ_author_name
'Mukherjee, Arindam'
'Nethaji, Munirathinam'
'Chakravarty, Akhil R.'
_publ_section_title
;
 Encapsulation of paramagnetic 3d1-vanadium(IV) in an
 antiferromagnetically coupled dodecanuclear copper(II) cage
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   24
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              2978
_journal_page_last               2979
_journal_paper_doi               10.1039/b310521k
_journal_year                    2003
_chemical_formula_moiety         'C104 H102 Cl6 Cu12 N12 O28 V1'
_chemical_formula_sum            'C104 H102 Cl6 Cu12 N12 O28 V'
_chemical_formula_weight         2994.10
_space_group_IT_number           167
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   16.001(3)
_cell_length_b                   16.001(3)
_cell_length_c                   79.15(4)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.56
_cell_measurement_theta_min      1.54
_cell_volume                     17550(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      273(2)
_diffrn_detector_area_resol_mean 0.03
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0447
_diffrn_reflns_av_sigmaI/netI    0.0311
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       101
_diffrn_reflns_limit_l_min       -100
_diffrn_reflns_number            43444
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    2.421
_exptl_absorpt_correction_T_max  0.94907
_exptl_absorpt_correction_T_min  0.69426
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.700
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             9042
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         2.577
_refine_diff_density_min         -1.098
_refine_diff_density_rms         0.217
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     239
_refine_ls_number_reflns         4318
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.147
_refine_ls_R_factor_all          0.0964
_refine_ls_R_factor_gt           0.0729
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1561P)²+49.2700P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2191
_refine_ls_wR_factor_ref         0.2494
_reflns_number_gt                3121
_reflns_number_total             4318
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7103913
_cod_data_source_file            b310521k.txt
_cod_data_source_block           '[Cu12VO5L6].2CHCl3.5H2O'
_cod_original_cell_volume        17552(9)
_cod_original_sg_symbol_H-M      R-3c
_cod_database_code               7113607
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'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'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'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'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-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'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-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'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
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
Cu1 Cu 0.77607(5) 0.56831(5) 0.080436(9) 0.0530(3) Uani 1 1 d .
Cu2 Cu 0.79279(5) 0.41662(5) 0.047605(8) 0.0482(3) Uani 1 1 d .
V1 V 0.6667 0.3333 0.0833 0.0378(5) Uani 1 6 d S
O5 O 0.5606(3) 0.2273(3) 0.0833 0.0424(11) Uani 1 2 d S
O3 O 0.7660(3) 0.3086(3) 0.03308(6) 0.0637(11) Uani 1 1 d .
O7 O 1.0000 0.0000 0.05470(10) 0.065(2) Uani 1 3 d S
O4 O 0.6667 0.3333 0.05814(8) 0.0404(13) Uani 1 3 d S
O2 O 0.8369(3) 0.5298(3) 0.06325(5) 0.0549(10) Uani 1 1 d .
O1 O 0.7237(3) 0.6065(3) 0.09848(6) 0.0667(12) Uani 1 1 d .
N2 N 0.9190(4) 0.4947(4) 0.03765(6) 0.0585(12) Uani 1 1 d .
N1 N 0.8758(4) 0.6965(4) 0.07574(8) 0.0689(15) Uani 1 1 d .
C15 C 0.8436(8) 0.2069(7) 0.00072(11) 0.097(3) Uani 1 1 d .
H15 H 0.8185 0.1500 -0.0055 0.116 Uiso 1 1 calc R
C2 C 0.6847(7) 0.7065(7) 0.11336(10) 0.086(2) Uani 1 1 d .
H2 H 0.6357 0.6534 0.1189 0.104 Uiso 1 1 calc R
C14 C 0.9385(7) 0.2797(7) -0.00215(11) 0.095(3) Uani 1 1 d .
H14 H 0.9770 0.2711 -0.0100 0.114 Uiso 1 1 calc R
C13 C 0.9728(6) 0.3616(6) 0.00650(10) 0.082(2) Uani 1 1 d .
H13 H 1.0362 0.4101 0.0046 0.099 Uiso 1 1 calc R
C16 C 0.7874(6) 0.2170(6) 0.01227(10) 0.081(2) Uani 1 1 d .
H16 H 0.7250 0.1662 0.0141 0.098 Uiso 1 1 calc R
C11 C 0.9605(5) 0.4686(5) 0.02678(9) 0.0668(17) Uani 1 1 d .
H11 H 1.0244 0.5127 0.0241 0.080 Uiso 1 1 calc R
C12 C 0.9171(5) 0.3776(5) 0.01834(7) 0.0635(16) Uani 1 1 d .
C17 C 0.8211(5) 0.3031(5) 0.02177(8) 0.0636(16) Uani 1 1 d .
C10 C 0.9747(5) 0.5900(5) 0.04547(10) 0.0700(18) Uani 1 1 d .
H10A H 1.0116 0.6382 0.0370 0.084 Uiso 1 1 calc R
H10B H 1.0192 0.5896 0.0538 0.084 Uiso 1 1 calc R
C7 C 0.8772(6) 0.7731(5) 0.08125(12) 0.082(2) Uani 1 1 d .
H7 H 0.9237 0.8315 0.0767 0.098 Uiso 1 1 calc R
C6 C 0.8157(7) 0.7773(6) 0.09345(12) 0.084(2) Uani 1 1 d .
C3 C 0.7020(10) 0.7995(10) 0.11709(15) 0.123(4) Uani 1 1 d .
H3 H 0.6624 0.8067 0.1248 0.147 Uiso 1 1 calc R
C1 C 0.7400(5) 0.6937(5) 0.10149(9) 0.0674(18) Uani 1 1 d .
C5 C 0.8322(10) 0.8696(8) 0.09840(17) 0.128(4) Uani 1 1 d .
H5 H 0.8837 0.9245 0.0937 0.154 Uiso 1 1 calc R
C8 C 0.9481(6) 0.7011(5) 0.06392(12) 0.087(2) Uani 1 1 d .
H8A H 1.0033 0.7071 0.0701 0.105 Uiso 1 1 calc R
H8B H 0.9701 0.7569 0.0566 0.105 Uiso 1 1 calc R
C4 C 0.7750(14) 0.8795(10) 0.1097(2) 0.161(7) Uani 1 1 d .
H4 H 0.7854 0.9405 0.1125 0.193 Uiso 1 1 calc R
C9 C 0.9044(3) 0.6126(4) 0.05382(8) 0.0699(18) Uani 1 1 d .
H9 H 0.8679 0.6217 0.0448 0.084 Uiso 1 1 calc R
Cl1 Cl 0.2193(3) 0.6047(4) 0.02032(8) 0.432(8) Uani 1 1 d R
C18 C 0.3333(3) 0.6667(4) 0.01076(8) 0.34(4) Uani 1 3 d SR
O8 O 1.1450(3) 0.0610(4) 0.02747(8) 0.273(16) Uiso 0.50 1 d PR
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'
V V 0.3005 0.5294 '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'
Cl Cl 0.1484 0.1585 '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 O1 93.8(2) . .
N1 Cu1 O5 173.9(2) . 3_665
O1 Cu1 O5 86.84(16) . 3_665
N1 Cu1 O2 85.5(2) . .
O1 Cu1 O2 175.6(2) . .
O5 Cu1 O2 94.26(14) 3_665 .
N2 Cu2 O3 91.6(2) . .
N2 Cu2 O4 177.33(19) . .
O3 Cu2 O4 87.26(17) . .
N2 Cu2 O2 83.5(2) . .
O3 Cu2 O2 172.69(19) . .
O4 Cu2 O2 97.40(17) . .
N2 Cu2 O3 105.4(2) . 2_655
O3 Cu2 O3 94.7(3) . 2_655
O4 Cu2 O3 77.08(16) . 2_655
O2 Cu2 O3 91.81(18) . 2_655
O5 V1 O5 120.000(1) 2_655 .
O5 V1 O5 120.000(2) 2_655 3_665
O5 V1 O5 120.000(1) . 3_665
O5 V1 O4 90.0 2_655 16_544
O5 V1 O4 90.0 . 16_544
O5 V1 O4 90.0 3_665 16_544
O5 V1 O4 90.0 2_655 .
O5 V1 O4 90.0 . .
O5 V1 O4 90.0 3_665 .
O4 V1 O4 180.0 16_544 .
V1 O5 Cu1 127.76(11) . 2_655
V1 O5 Cu1 127.76(11) . 17_554
Cu1 O5 Cu1 104.5(2) 2_655 17_554
C17 O3 Cu2 128.2(5) . .
C17 O3 Cu2 139.2(5) . 3_665
Cu2 O3 Cu2 91.84(16) . 3_665
Cu2 O4 Cu2 103.3(2) 3_665 .
Cu2 O4 Cu2 103.3(2) 3_665 2_655
Cu2 O4 Cu2 103.3(2) . 2_655
Cu2 O4 V1 115.13(17) 3_665 .
Cu2 O4 V1 115.13(17) . .
Cu2 O4 V1 115.13(17) 2_655 .
C9 O2 Cu1 109.7(3) . .
C9 O2 Cu2 106.0(3) . .
Cu1 O2 Cu2 135.4(2) . .
C1 O1 Cu1 126.5(5) . .
C11 N2 C10 118.7(5) . .
C11 N2 Cu2 127.5(5) . .
C10 N2 Cu2 113.3(4) . .
C7 N1 C8 122.1(6) . .
C7 N1 Cu1 124.4(6) . .
C8 N1 Cu1 113.3(4) . .
C16 C15 C14 121.6(8) . .
C1 C2 C3 120.1(10) . .
C13 C14 C15 118.7(7) . .
C14 C13 C12 122.5(8) . .
C15 C16 C17 121.6(8) . .
N2 C11 C12 125.6(6) . .
C13 C12 C17 119.6(7) . .
C13 C12 C11 118.0(7) . .
C17 C12 C11 122.4(6) . .
O3 C17 C16 119.5(7) . .
O3 C17 C12 124.4(7) . .
C16 C17 C12 116.1(6) . .
N2 C10 C9 107.4(5) . .
N1 C7 C6 126.7(7) . .
C7 C6 C5 118.0(9) . .
C7 C6 C1 123.2(7) . .
C5 C6 C1 118.7(9) . .
C4 C3 C2 122.0(10) . .
O1 C1 C2 119.0(8) . .
O1 C1 C6 122.8(7) . .
C2 C1 C6 118.2(7) . .
C4 C5 C6 121.6(13) . .
N1 C8 C9 108.5(6) . .
C5 C4 C3 119.3(11) . .
O2 C9 C8 112.7(5) . .
O2 C9 C10 108.5(5) . .
C8 C9 C10 114.9(5) . .
Cl1 C18 Cl1 102.76(10) 3_565 2_665
Cl1 C18 Cl1 102.8(3) 3_565 .
Cl1 C18 Cl1 102.8(2) 2_665 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N1 1.902(5) .
Cu1 O1 1.905(4) .
Cu1 O5 1.940(3) 3_665
Cu1 O2 1.943(4) .
Cu2 N2 1.934(5) .
Cu2 O3 1.937(4) .
Cu2 O4 1.963(3) .
Cu2 O2 2.008(4) .
Cu2 O3 2.331(4) 2_655
V1 O5 1.697(5) 2_655
V1 O5 1.697(5) .
V1 O5 1.697(5) 3_665
V1 O4 1.994(6) 16_544
V1 O4 1.994(6) .
O5 Cu1 1.940(3) 2_655
O5 Cu1 1.940(3) 17_554
O3 C17 1.291(7) .
O3 Cu2 2.331(4) 3_665
O4 Cu2 1.963(3) 3_665
O4 Cu2 1.963(3) 2_655
O2 C9 1.431(6) .
O1 C1 1.306(8) .
N2 C11 1.277(9) .
N2 C10 1.464(8) .
N1 C7 1.290(9) .
N1 C8 1.462(10) .
C15 C16 1.348(11) .
C15 C14 1.395(13) .
C2 C1 1.375(10) .
C2 C3 1.402(13) .
C14 C13 1.330(12) .
C13 C12 1.402(10) .
C16 C17 1.419(10) .
C11 C12 1.428(10) .
C12 C17 1.423(10) .
C10 C9 1.498(8) .
C7 C6 1.404(12) .
C6 C5 1.419(12) .
C6 C1 1.429(12) .
C3 C4 1.359(19) .
C5 C4 1.346(18) .
C8 C9 1.464(10) .
Cl1 C18 1.7535 .
C18 Cl1 1.754(8) 3_565
C18 Cl1 1.754(8) 2_665
