#------------------------------------------------------------------------------
#$Date: 2019-11-07 23:46:24 +0200 (Thu, 07 Nov 2019) $
#$Revision: 224101 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/90/7049027.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_7049027
loop_
_publ_author_name
'Passadis, Stamatis S.'
'Hadjithoma, Sofia'
'Kalampounias, Angelos G.'
'Tsipis, Athanassios C.'
'Sproules, Stephen'
'Miras, Haralampos N.'
'Keramidas, Anastasios D.'
'Kabanos, Themistoklis A.'
_publ_section_title
;
 Synthesis, structural and physicochemical characterization of a new type
 Ti₆-oxo cluster protected by a cyclic imide dioxime ligand.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5551
_journal_page_last               5559
_journal_paper_doi               10.1039/c9dt00658c
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C87 H128 K12 N36 O61 Ti12'
_chemical_formula_sum            'C87 H132 K12 N36 O61 Ti12'
_chemical_formula_weight         3697.74
_space_group_IT_number           163
_space_group_name_Hall           '-P 3 2c'
_space_group_name_H-M_alt        'P -3 1 c'
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3 2c'
_symmetry_space_group_name_H-M   'P -3 1 c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2018-11-29 deposited with the CCDC.    2019-02-14 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            1
_cell_length_a                   20.265(5)
_cell_length_b                   20.265(5)
_cell_length_c                   13.335(3)
_cell_measurement_reflns_used    8231
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.237
_cell_measurement_theta_min      2.317
_cell_volume                     4743(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω 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  0.1084
_diffrn_reflns_av_sigmaI/netI    0.0489
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            61400
_diffrn_reflns_theta_full        26.51
_diffrn_reflns_theta_max         26.51
_diffrn_reflns_theta_min         1.92
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.816
_exptl_absorpt_correction_T_max  0.9229
_exptl_absorpt_correction_T_min  0.8538
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1886
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.735
_refine_diff_density_min         -0.514
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         3215
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.1463
_refine_ls_R_factor_gt           0.0826
_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)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2615
_refine_ls_wR_factor_ref         0.3239
_reflns_number_gt                1612
_reflns_number_total             3215
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c9dt00658c2.cif
_cod_data_source_block           new
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7049027.cif.
;
_cod_original_cell_volume        4742.6(19)
_cod_original_sg_symbol_H-M      P-31c
_cod_database_code               7049027
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-y, -x, -z+1/2'
'-x+y, -x, z'
'x, x-y, -z+1/2'
'-x+y, y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'y, x, z-1/2'
'x-y, x, -z'
'-x, -x+y, z-1/2'
'x-y, -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
C1 C 0.9324(4) 0.4227(6) 0.3748(4) 0.073(2) Uani 1 1 d . A 1
C2 C 1.0022(5) 0.4161(6) 0.3707(5) 0.087(3) Uani 1 1 d . A 1
H2A H 1.0229 0.4195 0.4389 0.105 Uiso 1 1 calc R A 1
H2B H 1.0417 0.4573 0.3290 0.105 Uiso 1 1 calc R A 1
C3 C 0.9764(6) 0.3336(7) 0.3215(7) 0.112(4) Uani 1 1 d . . 1
H3A H 0.9636 0.3342 0.2500 0.134 Uiso 1 1 calc R . 1
H3B H 1.0196 0.3238 0.3246 0.134 Uiso 1 1 calc R . 1
C4 C 0.9096(6) 0.2710(7) 0.3736(7) 0.096(3) Uani 1 1 d . A 1
H4A H 0.9245 0.2644 0.4420 0.115 Uiso 1 1 calc R A 1
H4B H 0.8918 0.2226 0.3365 0.115 Uiso 1 1 calc R A 1
C5 C 0.8460(5) 0.2898(5) 0.3796(4) 0.067(2) Uani 1 1 d . A 1
C16 C 0.7862(6) 0.4480(6) 0.6120(5) 0.098(3) Uani 1 1 d . B 1
H16A H 0.8212 0.5005 0.5909 0.147 Uiso 1 1 calc R B 1
H16B H 0.7987 0.4404 0.6804 0.147 Uiso 1 1 calc R B 1
H16C H 0.7337 0.4384 0.6102 0.147 Uiso 1 1 calc R B 1
K1 K 0.90862(13) 0.36308(13) 0.62795(13) 0.0965(8) Uani 1 1 d . . 1
N1 N 0.9359(3) 0.4878(5) 0.3750(3) 0.0656(17) Uani 1 1 d . . 1
H1 H 0.9799 0.5305 0.3713 0.079 Uiso 1 1 calc R . 1
N2 N 0.8619(4) 0.3639(4) 0.3793(3) 0.0643(17) Uani 1 1 d . A 1
N3 N 0.7780(4) 0.2388(4) 0.3864(4) 0.0644(16) Uani 1 1 d . A 1
O5 O 0.7931(3) 0.3964(3) 0.5455(3) 0.0694(13) Uani 1 1 d . B 1
O1 O 0.8696(3) 0.4884(3) 0.3812(3) 0.0691(14) Uani 1 1 d . C 1
O2 O 0.7305(3) 0.2700(3) 0.4015(3) 0.0620(13) Uani 1 1 d . . 1
O3 O 0.6667 0.3333 0.4193(4) 0.0511(18) Uani 1 3 d S . 1
O4 O 0.7651(3) 0.38253(17) 0.2500 0.0538(15) Uani 1 2 d S . 1
O11 O 0.8488(12) 0.1911(10) 0.6534(16) 0.072(6) Uani 0.25 1 d P . 1
Ti1 Ti 0.77343(7) 0.38687(7) 0.38416(7) 0.0535(5) Uani 1 1 d . . 1
O6B O 0.0666(16) 0.3028(19) 0.561(2) 0.100(8) Uiso 0.25 1 d PD D 2
C10B C 0.004(3) 0.234(2) 0.596(4) 0.141(17) Uiso 0.25 1 d PD D 2
O6 O 0.1073(11) 0.3492(11) 0.5201(15) 0.058(4) Uiso 0.25 1 d PD E 3
C10 C 0.1125(19) 0.3272(18) 0.6173(17) 0.072(8) Uiso 0.25 1 d PD E 3
O6C O 0.0850(16) 0.3482(18) 0.572(2) 0.090(7) Uiso 0.25 1 d PD F 4
C10C C 0.091(4) 0.300(4) 0.500(5) 0.18(2) Uiso 0.25 1 d PD F 4
O7 O 0.9248(16) 0.1219(17) 0.248(3) 0.134(12) Uiso 0.25 1 d PD . .
C11 C 0.970(4) 0.130(5) 0.335(4) 0.20(3) Uiso 0.25 1 d PD . .
C20 C 0.8104(14) 0.1896(14) 0.7500 0.171(16) Uiso 0.50 2 d SP . .
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'
K K 0.2009 0.2494 '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'
Ti Ti 0.2776 0.4457 '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 C1 N2 113.7(7) . .
N1 C1 C2 121.8(8) . .
N2 C1 C2 124.5(9) . .
N1 C1 K1 106.1(4) . .
N2 C1 K1 75.4(3) . .
C2 C1 K1 88.7(4) . .
C1 C2 C3 106.2(8) . .
C1 C2 H2A 110.5 . .
C3 C2 H2A 110.5 . .
C1 C2 H2B 110.5 . .
C3 C2 H2B 110.5 . .
H2A C2 H2B 108.7 . .
C4 C3 C2 112.2(8) . .
C4 C3 K1 160.2(7) . 11_765
C2 C3 K1 79.6(5) . 11_765
C4 C3 H3A 109.2 . .
C2 C3 H3A 109.2 . .
K1 C3 H3A 51.1 11_765 .
C4 C3 H3B 109.2 . .
C2 C3 H3B 109.2 . .
K1 C3 H3B 80.0 11_765 .
H3A C3 H3B 107.9 . .
C3 C4 C5 109.6(8) . .
C3 C4 H4A 109.8 . .
C5 C4 H4A 109.8 . .
C3 C4 H4B 109.8 . .
C5 C4 H4B 109.8 . .
H4A C4 H4B 108.2 . .
N3 C5 N2 117.8(7) . .
N3 C5 C4 121.4(8) . .
N2 C5 C4 120.8(8) . .
O5 K1 O11 113.0(4) . .
O5 K1 N1 107.99(18) . 7_766
O11 K1 N1 137.7(4) . 7_766
O5 K1 N2 52.45(14) . .
O11 K1 N2 99.1(4) . .
N1 K1 N2 97.52(15) 7_766 .
O5 K1 C20 106.8(7) . .
O11 K1 C20 25.6(6) . .
N1 K1 C20 141.9(5) 7_766 .
N2 K1 C20 115.93(15) . .
O5 K1 C3 153.5(2) . 11_766
O11 K1 C3 76.9(5) . 11_766
N1 K1 C3 71.0(2) 7_766 11_766
N2 K1 C3 153.2(2) . 11_766
C20 K1 C3 71.0(4) . 11_766
O5 K1 C1 63.57(16) . .
O11 K1 C1 113.6(4) . .
N1 K1 C1 75.83(17) 7_766 .
N2 K1 C1 21.86(17) . .
C20 K1 C1 135.0(2) . .
C3 K1 C1 137.1(2) 11_766 .
O5 K1 K1 77.11(10) . 5_556
O11 K1 K1 128.9(4) . 5_556
N1 K1 K1 69.93(14) 7_766 5_556
N2 K1 K1 121.88(14) . 5_556
C20 K1 K1 103.6(5) . 5_556
C3 K1 K1 77.85(19) 11_766 5_556
C1 K1 K1 115.2(2) . 5_556
C1 N1 O1 117.7(7) . .
C1 N1 K1 120.7(5) . 7_766
O1 N1 K1 121.6(5) . 7_766
C1 N1 H1 121.1 . .
O1 N1 H1 121.1 . .
K1 N1 H1 2.6 7_766 .
C1 N2 C5 122.8(8) . .
C1 N2 Ti1 117.7(6) . .
C5 N2 Ti1 119.5(5) . .
C1 N2 K1 82.7(3) . .
C5 N2 K1 84.7(3) . .
Ti1 N2 K1 104.03(19) . .
C5 N3 O2 111.1(6) . .
C16 O5 Ti1 126.6(5) . .
C16 O5 K1 108.4(4) . .
Ti1 O5 K1 118.6(2) . .
N1 O1 Ti1 116.8(5) . .
N3 O2 Ti1 120.2(4) . .
N3 O2 Ti1 133.1(4) . 4_665
Ti1 O2 Ti1 101.9(2) . 4_665
Ti1 O3 Ti1 114.32(13) . 4_665
Ti1 O3 Ti1 114.32(13) . 2_655
Ti1 O3 Ti1 114.32(13) 4_665 2_655
Ti1 O4 Ti1 170.6(4) . 5
C20 O11 K1 91.4(14) . .
O4 Ti1 O3 99.3(3) . .
O4 Ti1 O1 92.9(2) . .
O3 Ti1 O1 145.28(19) . .
O4 Ti1 N2 91.67(19) . .
O3 Ti1 N2 137.4(2) . .
O1 Ti1 N2 73.9(3) . .
O4 Ti1 O2 94.53(14) . .
O3 Ti1 O2 67.76(14) . .
O1 Ti1 O2 143.7(2) . .
N2 Ti1 O2 70.4(2) . .
O4 Ti1 O2 94.71(14) . 2_655
O3 Ti1 O2 67.74(14) . 2_655
O1 Ti1 O2 79.0(2) . 2_655
N2 Ti1 O2 152.4(3) . 2_655
O2 Ti1 O2 135.4(2) . 2_655
O4 Ti1 O5 175.6(2) . .
O3 Ti1 O5 85.1(2) . .
O1 Ti1 O5 83.54(18) . .
N2 Ti1 O5 84.82(19) . .
O2 Ti1 O5 86.87(18) . .
O2 Ti1 O5 87.21(19) 2_655 .
O4 Ti1 Ti1 85.89(17) . 4_665
O3 Ti1 Ti1 32.84(7) . 4_665
O1 Ti1 Ti1 177.18(17) . 4_665
N2 Ti1 Ti1 108.7(2) . 4_665
O2 Ti1 Ti1 39.05(14) . 4_665
O2 Ti1 Ti1 98.53(14) 2_655 4_665
O5 Ti1 Ti1 97.80(14) . 4_665
O4 Ti1 Ti1 85.99(17) . 2_655
O3 Ti1 Ti1 32.84(7) . 2_655
O1 Ti1 Ti1 117.40(18) . 2_655
N2 Ti1 Ti1 168.5(2) . 2_655
O2 Ti1 Ti1 98.55(14) . 2_655
O2 Ti1 Ti1 39.02(14) 2_655 2_655
O5 Ti1 Ti1 97.98(14) . 2_655
Ti1 Ti1 Ti1 60.0 4_665 2_655
O7 O7 C11 110(6) 3_665 .
O11 C20 O11 129(4) 3_666 .
O11 C20 K1 141.7(9) 3_666 .
O11 C20 K1 62.9(10) . .
O11 C20 K1 62.9(10) 3_666 3_666
O11 C20 K1 141.7(9) . 3_666
K1 C20 K1 135.1(15) . 3_666
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.284(10) .
C1 N2 1.328(10) .
C1 C2 1.486(12) .
C1 K1 3.537(6) .
C2 C3 1.620(13) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 C4 1.486(14) .
C3 K1 3.519(9) 11_765
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C4 C5 1.518(12) .
C4 H4A 0.9900 .
C4 H4B 0.9900 .
C5 N3 1.245(11) .
C5 N2 1.371(10) .
C16 O5 1.430(11) .
C16 H16A 0.9800 .
C16 H16B 0.9800 .
C16 H16C 0.9800 .
K1 O5 2.954(6) .
K1 O11 3.082(18) .
K1 N1 3.089(7) 7_766
K1 N2 3.450(5) .
K1 C20 3.460(18) .
K1 C3 3.519(9) 11_766
K1 K1 4.926(5) 5_556
N1 O1 1.353(8) .
N1 K1 3.089(7) 7_766
N1 H1 0.8800 .
N2 Ti1 2.066(7) .
N3 O2 1.407(8) .
O5 Ti1 2.180(4) .
O1 Ti1 2.006(5) .
O2 Ti1 2.088(5) .
O2 Ti1 2.089(5) 4_665
O3 Ti1 1.9312(19) .
O3 Ti1 1.9312(19) 4_665
O3 Ti1 1.9312(19) 2_655
O4 Ti1 1.7951(11) .
O4 Ti1 1.7951(11) 5
O11 C20 1.50(3) .
Ti1 O2 2.089(5) 2_655
Ti1 Ti1 3.245(2) 4_665
Ti1 Ti1 3.245(2) 2_655
O6B C10B 1.42(2) .
O6 C10 1.391(18) .
O6C C10C 1.41(2) .
O7 O7 0.95(6) 3_665
O7 C11 1.44(2) .
C20 O11 1.50(3) 3_666
C20 K1 3.460(18) 3_666
