#------------------------------------------------------------------------------
#$Date: 2017-12-20 01:47:21 +0200 (Wed, 20 Dec 2017) $
#$Revision: 204365 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/68/4126874.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_4126874
loop_
_publ_author_name
'Luo, Dong'
'Wang, Xue-Zhi'
'Yang, Chen'
'Zhou, Xiao-Ping'
'Li, Dan'
_publ_section_title
;
 Self-Assembly of Chiral Metal-Organic Tetartoid.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b11285
_journal_year                    2017
_chemical_formula_sum            'C240 H272 B Co20 F4 N72 O16'
_chemical_formula_weight         5686.69
_space_group_crystal_system      cubic
_space_group_IT_number           196
_space_group_name_Hall           'F 2 2 3'
_space_group_name_H-M_alt        'F 2 3'
_symmetry_space_group_name_Hall  'F 2 2 3'
_symmetry_space_group_name_H-M   'F 2 3'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   33.0237(3)
_cell_length_b                   33.0237(3)
_cell_length_c                   33.0237(3)
_cell_measurement_reflns_used    5262
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.6300
_cell_measurement_theta_min      3.7730
_cell_volume                     36014.5(6)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0212
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            9346
_diffrn_reflns_point_group_measured_fraction_full 0.854
_diffrn_reflns_point_group_measured_fraction_max 0.823
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.975
_diffrn_reflns_theta_min         3.786
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    7.432
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44383
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.049
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             11700
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.543
_refine_diff_density_min         -0.461
_refine_diff_density_rms         0.104
_refine_ls_abs_structure_details
;
 Flack x determined using 1507 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.002(7)
_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     272
_refine_ls_number_reflns         4812
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0745
_refine_ls_R_factor_gt           0.0687
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1426P)²+151.9274P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1938
_refine_ls_wR_factor_ref         0.2026
_reflns_Friedel_coverage         0.626
_reflns_Friedel_fraction_full    0.710
_reflns_Friedel_fraction_max     0.671
_reflns_number_gt                4333
_reflns_number_total             4812
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja7b11285_si_002.cif
_cod_data_source_block           delta-2
_cod_original_cell_volume        36014.4(9)
_cod_database_code               4126874
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'z, x, y'
'y, z, x'
'-y, -z, x'
'z, -x, -y'
'-y, z, -x'
'-z, -x, y'
'-z, x, -y'
'y, -z, -x'
'-x, -y, z'
'x, -y, -z'
'-x, y, -z'
'x, y+1/2, z+1/2'
'z, x+1/2, y+1/2'
'y, z+1/2, x+1/2'
'-y, -z+1/2, x+1/2'
'z, -x+1/2, -y+1/2'
'-y, z+1/2, -x+1/2'
'-z, -x+1/2, y+1/2'
'-z, x+1/2, -y+1/2'
'y, -z+1/2, -x+1/2'
'-x, -y+1/2, z+1/2'
'x, -y+1/2, -z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, y, z+1/2'
'z+1/2, x, y+1/2'
'y+1/2, z, x+1/2'
'-y+1/2, -z, x+1/2'
'z+1/2, -x, -y+1/2'
'-y+1/2, z, -x+1/2'
'-z+1/2, -x, y+1/2'
'-z+1/2, x, -y+1/2'
'y+1/2, -z, -x+1/2'
'-x+1/2, -y, z+1/2'
'x+1/2, -y, -z+1/2'
'-x+1/2, y, -z+1/2'
'x+1/2, y+1/2, z'
'z+1/2, x+1/2, y'
'y+1/2, z+1/2, x'
'-y+1/2, -z+1/2, x'
'z+1/2, -x+1/2, -y'
'-y+1/2, z+1/2, -x'
'-z+1/2, -x+1/2, y'
'-z+1/2, x+1/2, -y'
'y+1/2, -z+1/2, -x'
'-x+1/2, -y+1/2, z'
'x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -z'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Co1 Co 0.64325(3) 0.85675(3) 0.14325(3) 0.0291(4) Uani 1 3 d S T P
Co3 Co 0.63851(5) 1.13851(5) 0.13851(5) 0.0475(6) Uani 1 3 d S T P
Co2 Co 0.54579(4) 0.99416(4) 0.21519(4) 0.0400(4) Uani 1 1 d . . .
O1 O 0.5000 1.0000 0.1719(2) 0.0302(13) Uani 1 2 d S T P
O2 O 0.5000 1.0000 0.2523(2) 0.0442(17) Uani 1 2 d S T P
N5 N 0.58016(18) 1.04342(19) 0.19937(18) 0.0341(13) Uani 1 1 d . . .
N4 N 0.59433(19) 0.99131(18) 0.26017(18) 0.0373(14) Uani 1 1 d . . .
N6 N 0.61783(19) 1.09301(19) 0.17312(19) 0.0381(14) Uani 1 1 d . . .
N2 N 0.60266(16) 0.89230(16) 0.16601(17) 0.0261(11) Uani 1 1 d . . .
N3 N 0.56014(17) 0.93718(17) 0.19306(17) 0.0300(12) Uani 1 1 d . . .
C5 C 0.5918(2) 0.9310(2) 0.1663(2) 0.0322(15) Uani 1 1 d . . .
C10 C 0.5821(2) 1.0735(2) 0.1728(2) 0.0332(15) Uani 1 1 d . . .
C12 C 0.6178(2) 1.0431(2) 0.2182(2) 0.0380(16) Uani 1 1 d . . .
C9 C 0.6410(3) 1.0730(3) 0.2024(3) 0.0471(19) Uani 1 1 d . . .
C7 C 0.6072(2) 0.9652(2) 0.1409(2) 0.0396(17) Uani 1 1 d . . .
H7A H 0.6360 0.9629 0.1380 0.059 Uiso 1 1 calc R U .
H7B H 0.6007 0.9905 0.1538 0.059 Uiso 1 1 calc R U .
H7C H 0.5947 0.9642 0.1147 0.059 Uiso 1 1 calc R U .
C11 C 0.5481(2) 1.0846(3) 0.1462(3) 0.0452(18) Uani 1 1 d . . .
H11A H 0.5555 1.0798 0.1185 0.068 Uiso 1 1 calc R U .
H11B H 0.5417 1.1127 0.1498 0.068 Uiso 1 1 calc R U .
H11C H 0.5248 1.0685 0.1530 0.068 Uiso 1 1 calc R U .
C13 C 0.6234(3) 1.0154(2) 0.2517(2) 0.0407(17) Uani 1 1 d . . .
H13 H 0.6473 1.0151 0.2666 0.049 Uiso 1 1 calc R U .
C8 C 0.6845(3) 1.0847(5) 0.2109(5) 0.088(4) Uani 1 1 d . . .
H8A H 0.6960 1.0971 0.1873 0.132 Uiso 1 1 calc R U .
H8B H 0.6997 1.0610 0.2179 0.132 Uiso 1 1 calc R U .
H8C H 0.6852 1.1036 0.2331 0.132 Uiso 1 1 calc R U .
C3 C 0.5787(2) 0.8730(2) 0.19311(19) 0.0266(13) Uani 1 1 d . . .
C6 C 0.5190(2) 0.8948(2) 0.2408(2) 0.0388(17) Uani 1 1 d . . .
H6A H 0.5243 0.9114 0.2641 0.058 Uiso 1 1 calc R U .
H6B H 0.5180 0.8669 0.2488 0.058 Uiso 1 1 calc R U .
H6C H 0.4935 0.9024 0.2291 0.058 Uiso 1 1 calc R U .
C4 C 0.5520(2) 0.90053(19) 0.2102(2) 0.0288(14) Uani 1 1 d . . .
O3 O 0.6735(2) 1.1735(2) 0.1735(2) 0.052(2) Uani 1 3 d S T P
H3A H 0.6628 0.2054 0.2092 0.077 Uiso 0.3333 1 d R U P
H3B H 0.7133 0.1793 0.1845 0.077 Uiso 0.3333 1 d R U P
C2 C 0.5883(2) 0.8314(2) 0.2008(2) 0.0276(13) Uani 1 1 d . . .
H2 H 0.5729 0.8153 0.2179 0.033 Uiso 1 1 calc R U .
N1 N 0.61999(17) 0.81787(16) 0.18216(16) 0.0278(12) Uani 1 1 d . . .
C16 C 0.6426(2) 0.9148(2) 0.2587(2) 0.0324(14) Uani 1 1 d . . .
H16 H 0.6535 0.9357 0.2433 0.039 Uiso 1 1 calc R U .
C19 C 0.6400(2) 0.8443(2) 0.2761(2) 0.0362(16) Uani 1 1 d . . .
H19 H 0.6495 0.8180 0.2727 0.043 Uiso 1 1 calc R U .
C14 C 0.5991(3) 0.9655(2) 0.2962(2) 0.0408(17) Uani 1 1 d . . .
H14A H 0.5734 0.9645 0.3105 0.049 Uiso 1 1 calc R U .
H14B H 0.6188 0.9777 0.3141 0.049 Uiso 1 1 calc R U .
C20 C 0.6567(2) 0.8750(2) 0.2536(2) 0.0318(14) Uani 1 1 d . . .
C18 C 0.6097(2) 0.8517(2) 0.3035(2) 0.0366(16) Uani 1 1 d . . .
H18 H 0.5985 0.8306 0.3183 0.044 Uiso 1 1 calc R U .
C1 C 0.6337(2) 0.77611(19) 0.1906(2) 0.0297(14) Uani 1 1 d . . .
H1A H 0.6206 0.7666 0.2151 0.036 Uiso 1 1 calc R U .
H1B H 0.6627 0.7765 0.1956 0.036 Uiso 1 1 calc R U .
C17 C 0.5957(2) 0.8911(2) 0.3089(2) 0.0360(15) Uani 1 1 d . . .
H17 H 0.5752 0.8962 0.3274 0.043 Uiso 1 1 calc R U .
C15 C 0.6122(2) 0.9229(2) 0.2868(2) 0.0363(15) Uani 1 1 d . . .
B1 B 0.7500 0.7500 0.2500 0.034(6) Uani 1 12 d S T P
F1 F 0.7275(3) 0.7725(3) 0.2725(3) 0.159(8) Uani 1 3 d S T P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co -2.3653 3.6143 '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
N2 Co1 N2 94.9(2) 28_664 41_566
N2 Co1 N2 94.9(2) 28_664 .
N2 Co1 N2 94.9(2) 41_566 .
N2 Co1 N1 176.5(2) 28_664 41_566
N2 Co1 N1 82.6(2) 41_566 41_566
N2 Co1 N1 87.8(2) . 41_566
N2 Co1 N1 82.6(2) 28_664 28_664
N2 Co1 N1 87.8(2) 41_566 28_664
N2 Co1 N1 176.5(2) . 28_664
N1 Co1 N1 94.8(2) 41_566 28_664
N2 Co1 N1 87.8(2) 28_664 .
N2 Co1 N1 176.5(2) 41_566 .
N2 Co1 N1 82.6(2) . .
N1 Co1 N1 94.8(2) 41_566 .
N1 Co1 N1 94.8(2) 28_664 .
O3 Co3 N6 107.5(2) . .
O3 Co3 N6 107.5(2) . 38_554
N6 Co3 N6 111.41(19) . 38_554
O3 Co3 N6 107.5(2) . 27_464
N6 Co3 N6 111.41(19) . 27_464
N6 Co3 N6 111.41(19) 38_554 27_464
O2 Co2 N5 120.61(18) . .
O2 Co2 N3 119.14(18) . .
N5 Co2 N3 120.2(2) . .
O2 Co2 O1 82.0(2) . .
N5 Co2 O1 98.80(19) . .
N3 Co2 O1 90.46(18) . .
O2 Co2 N4 98.4(3) . .
N5 Co2 N4 78.6(2) . .
N3 Co2 N4 91.9(2) . .
O1 Co2 N4 177.12(18) . .
Co2 O1 Co2 93.7(3) 10_675 .
Co2 O2 Co2 102.4(4) 10_675 .
C10 N5 C12 105.0(6) . .
C10 N5 Co2 142.0(5) . .
C12 N5 Co2 112.1(5) . .
C13 N4 C14 117.2(7) . .
C13 N4 Co2 112.1(5) . .
C14 N4 Co2 130.6(5) . .
C10 N6 C9 105.0(6) . .
C10 N6 Co3 130.7(5) . .
C9 N6 Co3 124.1(5) . .
C5 N2 C3 106.8(6) . .
C5 N2 Co1 140.8(5) . .
C3 N2 Co1 112.1(4) . .
C4 N3 C5 106.4(5) . .
C4 N3 Co2 127.9(5) . .
C5 N3 Co2 122.1(5) . .
N2 C5 N3 110.6(6) . .
N2 C5 C7 129.0(6) . .
N3 C5 C7 120.2(6) . .
N5 C10 N6 113.3(6) . .
N5 C10 C11 123.0(7) . .
N6 C10 C11 123.8(7) . .
C9 C12 N5 109.2(7) . .
C9 C12 C13 133.1(8) . .
N5 C12 C13 117.4(7) . .
C12 C9 N6 107.5(7) . .
C12 C9 C8 130.7(9) . .
N6 C9 C8 121.8(8) . .
N4 C13 C12 117.6(7) . .
N2 C3 C4 109.5(6) . .
N2 C3 C2 116.0(6) . .
C4 C3 C2 134.3(6) . .
N3 C4 C3 106.7(6) . .
N3 C4 C6 122.4(6) . .
C3 C4 C6 130.9(6) . .
N1 C2 C3 115.3(6) . .
C2 N1 C1 118.8(6) . .
C2 N1 Co1 113.5(4) . .
C1 N1 Co1 127.7(4) . .
C15 C16 C20 119.8(6) . .
C18 C19 C20 121.1(7) . .
N4 C14 C15 114.0(6) . .
C19 C20 C16 119.7(7) . .
C19 C20 C1 120.3(6) . 41_566
C16 C20 C1 120.0(6) . 41_566
C19 C18 C17 119.5(7) . .
N1 C1 C20 113.9(5) . 28_664
C15 C17 C18 120.6(7) . .
C17 C15 C16 119.2(7) . .
C17 C15 C14 119.0(7) . .
C16 C15 C14 121.6(7) . .
F1 B1 F1 109.471(3) . 28_664
F1 B1 F1 109.471(2) . 26_554
F1 B1 F1 109.471(1) 28_664 26_554
F1 B1 F1 109.471(6) . 15_554
F1 B1 F1 109.471(3) 28_664 15_554
F1 B1 F1 109.471(10) 26_554 15_554
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 N2 1.934(5) 28_664
Co1 N2 1.934(5) 41_566
Co1 N2 1.934(5) .
Co1 N1 1.972(6) 41_566
Co1 N1 1.972(6) 28_664
Co1 N1 1.972(6) .
Co3 O3 2.003(12) .
Co3 N6 2.008(6) .
Co3 N6 2.008(6) 38_554
Co3 N6 2.008(6) 27_464
Co2 O2 1.956(5) .
Co2 N5 2.051(6) .
Co2 N3 2.074(6) .
Co2 O1 2.090(5) .
Co2 N4 2.187(6) .
O1 Co2 2.090(5) 10_675
O2 Co2 1.956(5) 10_675
N5 C10 1.327(10) .
N5 C12 1.389(10) .
N4 C13 1.277(10) .
N4 C14 1.472(9) .
N6 C10 1.345(10) .
N6 C9 1.398(11) .
N2 C5 1.328(9) .
N2 C3 1.353(9) .
N3 C4 1.363(8) .
N3 C5 1.382(9) .
C5 C7 1.496(11) .
C10 C11 1.471(10) .
C12 C9 1.353(12) .
C12 C13 1.450(11) .
C9 C8 1.513(14) .
C3 C4 1.386(9) .
C3 C2 1.433(9) .
C6 C4 1.499(10) .
C2 N1 1.292(9) .
N1 C1 1.478(8) .
C16 C15 1.393(11) .
C16 C20 1.404(10) .
C19 C18 1.372(10) .
C19 C20 1.372(10) .
C14 C15 1.504(10) .
C20 C1 1.518(10) 41_566
C18 C17 1.392(11) .
C1 C20 1.518(10) 28_664
C17 C15 1.389(11) .
B1 F1 1.285(17) .
B1 F1 1.285(17) 28_664
B1 F1 1.285(17) 26_554
B1 F1 1.285(17) 15_554
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.001 -0.004 -0.001 15007 3091 ' '
2 0.500 0.000 0.000 394 166 ' '
3 0.000 0.000 0.500 394 166 ' '
4 0.000 0.500 0.000 394 166 ' '
5 0.500 0.500 0.500 394 166 ' '
