#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:58:59 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179087 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/49/4304912.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_4304912
loop_
_publ_author_name
'Sanjit Konar'
'Abraham Clearfield'
_publ_contact_author
; 
'Abraham Clearfield'
;
_publ_contact_author_email       clearfield@mail.chem.tamu.edu
_publ_contact_author_phone       '+1 979 997 9299'
_publ_section_title
;
Mixed-Valent Dodecanuclear Vanadium Cluster Encapsulating Chloride Anions
and Its Reaction To Form a "Bowl"-Shaped Cluster
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3492
_journal_page_last               3494
_journal_paper_doi               10.1021/ic800013f
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C117 H75 Cl5 N6 O52 P6 V12'
_chemical_formula_weight         3371.18
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           190
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P -6c -2c'
_symmetry_space_group_name_H-M   'P -6 2 c'
_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            2
_cell_length_a                   16.8442(16)
_cell_length_b                   16.8442(16)
_cell_length_c                   34.778(7)
_cell_measurement_temperature    110(2)
_cell_volume                     8545(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0327
_diffrn_reflns_av_sigmaI/netI    0.0145
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            69116
_diffrn_reflns_theta_full        23.38
_diffrn_reflns_theta_max         23.38
_diffrn_reflns_theta_min         1.40
_exptl_absorpt_coefficient_mu    0.830
_exptl_absorpt_correction_T_max  0.868
_exptl_absorpt_correction_T_min  0.847
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS V2.10'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             3372
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.707
_refine_diff_density_min         -0.885
_refine_diff_density_rms         0.293
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.04(5)
_refine_ls_extinction_coef       0.0058(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.186
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         4250
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.186
_refine_ls_R_factor_all          0.0735
_refine_ls_R_factor_gt           0.0632
_refine_ls_shift/su_max          1.089
_refine_ls_shift/su_mean         0.142
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1368P)²+8.2902P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1809
_refine_ls_wR_factor_ref         0.1976
_reflns_number_gt                3977
_reflns_number_total             4250
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800013f-file003.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Hexagonal' changed to 'hexagonal'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-Scan' changed
to 'multi-scan' 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_cell_volume        8546(2)
_cod_database_code               4304912
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x, y, -z+1/2'
'-y, x-y, -z+1/2'
'-x+y, -x, -z+1/2'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'y, x, z+1/2'
'x-y, -y, z+1/2'
'-x, -x+y, 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_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
V1 V -0.20434(8) 0.53163(8) 0.35926(3) 0.0413(4) Uani 1 1 d . . .
V2 V -0.30608(8) 0.45771(8) 0.44649(3) 0.0453(4) Uani 1 1 d . . .
Cl1 Cl 0.3333 0.6667 0.62015(6) 0.0375(6) Uani 1 3 d S . .
Cl2 Cl 0.84336(14) 0.39381(15) 0.2500 0.0407(5) Uani 1 2 d S . .
P5 P -0.10607(11) 0.40877(13) 0.37241(5) 0.0429(4) Uani 1 1 d . . .
O4 O -0.2160(3) 0.5336(3) 0.40767(12) 0.0466(11) Uani 1 1 d . . .
O8 O -0.1239(3) 0.4825(3) 0.35605(11) 0.0425(11) Uani 1 1 d . . .
O7 O -0.2386(3) 0.4117(3) 0.46160(12) 0.0483(11) Uani 1 1 d . . .
O3 O -0.2354(3) 0.4774(3) 0.30412(11) 0.0480(11) Uani 1 1 d . . .
O1 O -0.3204(4) 0.5246(3) 0.34893(13) 0.0475(11) Uani 1 1 d . . .
O5 O -0.3915(3) 0.4802(3) 0.41474(12) 0.0472(11) Uani 1 1 d . . .
O6 O -0.2903(4) 0.5277(4) 0.47970(14) 0.0582(13) Uani 1 1 d . . .
O2 O -0.1342(4) 0.6344(4) 0.34895(14) 0.0574(13) Uani 1 1 d . . .
C4 C 0.1758(5) 0.6094(6) 0.4450(2) 0.059(2) Uani 1 1 d . . .
H4 H 0.2109 0.6069 0.4651 0.071 Uiso 1 1 calc R . .
C6 C 0.0734(5) 0.5370(6) 0.3911(2) 0.0562(18) Uani 1 1 d . . .
C1 C 0.0766(6) 0.6173(5) 0.3829(2) 0.063(2) Uani 1 1 d . . .
H1 H 0.0441 0.6214 0.3620 0.075 Uiso 1 1 calc R . .
C5 C 0.1216(5) 0.5308(5) 0.4225(2) 0.0560(18) Uani 1 1 d . . .
H5 H 0.1180 0.4754 0.4285 0.067 Uiso 1 1 calc R . .
C3 C 0.1764(6) 0.6882(6) 0.4372(2) 0.069(2) Uani 1 1 d . . .
H3 H 0.2089 0.7390 0.4530 0.083 Uiso 1 1 calc R . .
C22 C 0.0184(6) 0.4523(7) 0.3656(3) 0.076(3) Uani 1 1 d . . .
C2 C 0.1294(6) 0.6941(6) 0.4061(3) 0.075(3) Uani 1 1 d . . .
H2 H 0.1326 0.7496 0.4003 0.090 Uiso 1 1 calc R . .
C12A C 0.1137(8) 0.4006(12) 0.3352(3) 0.104(4) Uani 1 1 d . . .
C7A C 0.0470(9) 0.3851(10) 0.3602(4) 0.045(3) Uani 0.521(11) 1 d P . .
C8A C 0.0153(10) 0.3114(11) 0.3840(4) 0.060(4) Uani 0.521(11) 1 d P . .
C9A C 0.0438(16) 0.2474(13) 0.3834(7) 0.086(7) Uani 0.521(11) 1 d P . .
C10A C 0.1042(15) 0.2548(15) 0.3586(7) 0.082(7) Uani 0.521(11) 1 d P . .
C11A C 0.1389(16) 0.325(2) 0.3325(6) 0.102(9) Uani 0.521(11) 1 d P . .
C7B C 0.0558(11) 0.445(2) 0.3383(5) 0.080(8) Uani 0.479(11) 1 d P . .
C8B C 0.0367(16) 0.470(2) 0.3058(6) 0.100(9) Uani 0.479(11) 1 d P . .
C9B C 0.086(2) 0.475(3) 0.2693(7) 0.145(15) Uani 0.479(11) 1 d P . .
C10B C 0.140(2) 0.446(3) 0.2718(9) 0.154(17) Uani 0.479(11) 1 d P . .
C11B C 0.160(3) 0.413(6) 0.3059(8) 0.29(5) Uani 0.479(11) 1 d P . .
N1 N 0.5513(9) 1.0000 0.5000 0.136(8) Uani 1 2 d S . .
H1A H 0.5002 1.0000 0.5000 0.164 Uiso 1 2 calc SR . .
C16 C 0.7061(10) 1.0000 0.5000 0.096(4) Uani 1 2 d S . .
H16 H 0.7613 1.0000 0.5000 0.115 Uiso 1 2 calc SR . .
C14 C 0.6416(9) 0.9550(7) 0.5272(3) 0.083(3) Uani 1 1 d . . .
H14 H 0.6539 0.9226 0.5457 0.100 Uiso 1 1 calc R . .
C15 C 0.5685(8) 0.9535(7) 0.5294(3) 0.078(3) Uani 1 1 d . . .
H15 H 0.5270 0.9237 0.5492 0.094 Uiso 1 1 calc R . .
C43 C 0.8137(10) 0.7536(10) 0.2891(3) 0.103(4) Uani 1 1 d . . .
H43 H 0.8150 0.7531 0.3158 0.124 Uiso 1 1 calc R . .
C41 C 0.8663(8) 0.8300(7) 0.2695(4) 0.101(4) Uani 1 1 d . . .
H41 H 0.9036 0.8842 0.2827 0.121 Uiso 1 1 calc R . .
C42 C 0.7593(9) 0.6780(7) 0.2694(3) 0.095(3) Uani 1 1 d . . .
H42 H 0.7205 0.6242 0.2825 0.114 Uiso 1 1 calc R . .
O2W O 0.3333 0.6667 0.3565(4) 0.154(8) Uani 1 3 d S . .
O3W O 0.0000 0.0000 0.67425(17) 0.0342(14) Uani 1 3 d S . .
C45 C 1.0073(17) 0.742(2) 0.2500 0.29(3) Uani 1 2 d S . .
C44 C 0.9653(17) 0.6507(16) 0.2500 0.180(14) Uani 1 2 d S . .
H44A H 0.9272 0.6274 0.2724 0.270 Uiso 0.50 1 calc PR . .
H44B H 1.0103 0.6317 0.2502 0.270 Uiso 1 2 calc SR . .
H44C H 0.9282 0.6274 0.2273 0.270 Uiso 0.50 1 calc PR . .
N3 N 1.022(2) 0.822(2) 0.2500 0.40(3) Uani 1 2 d S . .
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'
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'
H H 0.0000 0.0000 '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
O2 V1 O4 103.6(2) . . ?
O2 V1 O8 99.1(3) . . ?
O4 V1 O8 100.4(2) . . ?
O2 V1 O1 101.8(3) . . ?
O4 V1 O1 93.6(2) . . ?
O8 V1 O1 151.3(2) . . ?
O2 V1 O3 99.1(2) . . ?
O4 V1 O3 156.8(2) . . ?
O8 V1 O3 80.37(18) . . ?
O1 V1 O3 77.11(19) . . ?
O6 V2 O7 102.0(3) . . ?
O6 V2 O7 104.1(2) . 2_565 ?
O7 V2 O7 89.9(3) . 2_565 ?
O6 V2 O4 103.4(2) . . ?
O7 V2 O4 91.9(2) . . ?
O7 V2 O4 151.42(19) 2_565 . ?
O6 V2 O5 97.6(2) . . ?
O7 V2 O5 160.4(2) . . ?
O7 V2 O5 85.1(2) 2_565 . ?
O4 V2 O5 83.8(2) . . ?
O5 P5 O1 111.9(3) 3_455 3_455 ?
O5 P5 O8 112.9(3) 3_455 . ?
O1 P5 O8 111.4(3) 3_455 . ?
O5 P5 C22 108.7(4) 3_455 . ?
O1 P5 C22 105.6(4) 3_455 . ?
O8 P5 C22 105.9(4) . . ?
V1 O4 V2 137.0(3) . . ?
P5 O8 V1 143.2(3) . . ?
V2 O7 V2 131.6(3) . 3_455 ?
P5 O1 V1 131.5(3) 2_565 . ?
P5 O5 V2 136.6(3) 2_565 . ?
C3 C4 C5 119.6(7) . . ?
C1 C6 C5 120.4(8) . . ?
C1 C6 C22 120.6(8) . . ?
C5 C6 C22 119.0(8) . . ?
C6 C1 C2 119.2(8) . . ?
C6 C5 C4 119.5(7) . . ?
C2 C3 C4 120.5(8) . . ?
C7B C22 C7A 53.7(15) . . ?
C7B C22 C6 117.3(13) . . ?
C7A C22 C6 121.4(8) . . ?
C7B C22 P5 128.0(11) . . ?
C7A C22 P5 117.3(8) . . ?
C6 C22 P5 109.3(6) . . ?
C3 C2 C1 120.7(8) . . ?
C11B C12A C7A 165.3(16) . . ?
C11B C12A C7B 120(3) . . ?
C7A C12A C7B 50.2(11) . . ?
C11B C12A C11A 71(4) . . ?
C7A C12A C11A 115.5(17) . . ?
C7B C12A C11A 159.5(18) . . ?
C7B C7A C8A 166.1(16) . . ?
C7B C7A C12A 71.7(14) . . ?
C8A C7A C12A 118.8(14) . . ?
C7B C7A C22 51.9(12) . . ?
C8A C7A C22 120.2(13) . . ?
C12A C7A C22 120.4(14) . . ?
C7A C8A C9A 124.9(18) . . ?
C10A C9A C8A 120(2) . . ?
C9A C10A C11A 120.4(17) . . ?
C10A C11A C12A 120.0(16) . . ?
C10A C11A C11B 165.5(19) . . ?
C12A C11A C11B 46.1(16) . . ?
C22 C7B C7A 74.5(14) . . ?
C22 C7B C8B 116(2) . . ?
C7A C7B C8B 150(2) . . ?
C22 C7B C12A 129(2) . . ?
C7A C7B C12A 58.2(16) . . ?
C8B C7B C12A 115.1(17) . . ?
C7B C8B C9B 123(2) . . ?
C10B C9B C9B 94.2(19) . 4 ?
C10B C9B C8B 114(3) . . ?
C9B C9B C8B 148.1(14) 4 . ?
C10B C9B C10B 54(2) . 4 ?
C9B C9B C10B 40.6(12) 4 4 ?
C8B C9B C10B 162(3) . 4 ?
C9B C10B C11B 126(3) . . ?
C9B C10B C10B 85.8(19) . 4 ?
C11B C10B C10B 146(3) . 4 ?
C9B C10B C9B 45(2) . 4 ?
C11B C10B C9B 168(3) . 4 ?
C10B C10B C9B 40.6(12) 4 4 ?
C12A C11B C10B 119(3) . . ?
C12A C11B C11A 63(3) . . ?
C10B C11B C11A 148(5) . . ?
C15 N1 C15 122.0(14) . 8_676 ?
C14 C16 C14 116.9(17) . 8_676 ?
C15 C14 C16 125.1(13) . . ?
C14 C15 N1 115.5(12) . . ?
C41 C43 C42 118.1(11) . . ?
C43 C41 C41 120.9(7) . 4 ?
C43 C42 C42 121.0(8) . 4 ?
N3 C45 C44 163(3) . . ?
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
V1 O2 1.574(5) . ?
V1 O4 1.697(4) . ?
V1 O8 1.912(5) . ?
V1 O1 1.933(5) . ?
V1 O3 2.075(4) . ?
V2 O6 1.575(5) . ?
V2 O7 1.746(5) . ?
V2 O7 1.875(5) 2_565 ?
V2 O4 1.955(5) . ?
V2 O5 1.995(5) . ?
P5 O5 1.511(5) 3_455 ?
P5 O1 1.527(5) 3_455 ?
P5 O8 1.526(5) . ?
P5 C22 1.858(9) . ?
O7 V2 1.875(5) 3_455 ?
O1 P5 1.527(5) 2_565 ?
O5 P5 1.511(5) 2_565 ?
C4 C3 1.351(13) . ?
C4 C5 1.410(11) . ?
C6 C1 1.357(12) . ?
C6 C5 1.395(11) . ?
C6 C22 1.535(12) . ?
C1 C2 1.402(12) . ?
C3 C2 1.374(13) . ?
C22 C7B 1.182(19) . ?
C22 C7A 1.448(17) . ?
C12A C11B 1.24(3) . ?
C12A C7A 1.340(18) . ?
C12A C7B 1.50(3) . ?
C12A C11A 1.54(3) . ?
C7A C7B 1.21(3) . ?
C7A C8A 1.36(2) . ?
C8A C9A 1.38(2) . ?
C9A C10A 1.29(3) . ?
C10A C11A 1.36(4) . ?
C11A C11B 1.63(8) . ?
C7B C8B 1.30(3) . ?
C8B C9B 1.50(3) . ?
C9B C10B 1.23(5) . ?
C9B C9B 1.34(5) 4 ?
C9B C10B 1.88(4) 4 ?
C10B C11B 1.43(6) . ?
C10B C10B 1.52(6) 4 ?
C10B C9B 1.88(4) 4 ?
N1 C15 1.403(12) . ?
N1 C15 1.403(13) 8_676 ?
C16 C14 1.352(15) . ?
C16 C14 1.352(15) 8_676 ?
C14 C15 1.223(16) . ?
C43 C41 1.329(18) . ?
C43 C42 1.328(17) . ?
C41 C41 1.35(3) 4 ?
C42 C42 1.35(2) 4 ?
C45 N3 1.24(4) . ?
C45 C44 1.33(4) . ?
