#------------------------------------------------------------------------------
#$Date: 2017-12-20 01:47:21 +0200 (Wed, 20 Dec 2017) $
#$Revision: 204365 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/68/4126878.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_4126878
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            'C216 H224 Co20 F42 N72 O16 P7'
_chemical_formula_weight         6278.05
_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                   32.9732(2)
_cell_length_b                   32.9732(2)
_cell_length_c                   32.9732(2)
_cell_measurement_reflns_used    4288
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69.8890
_cell_measurement_theta_min      4.6140
_cell_volume                     35849.5(4)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_unetI/netI     0.0576
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            10465
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.567
_diffrn_reflns_theta_min         2.680
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    7.955
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.67659
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.163
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             12700
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.214
_refine_diff_density_min         -0.946
_refine_diff_density_rms         0.208
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.18(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.793
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     288
_refine_ls_number_reflns         5060
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.793
_refine_ls_R_factor_all          0.1684
_refine_ls_R_factor_gt           0.1568
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4104
_refine_ls_wR_factor_ref         0.4236
_reflns_Friedel_coverage         0.898
_reflns_Friedel_fraction_full    0.985
_reflns_Friedel_fraction_max     0.963
_reflns_number_gt                4148
_reflns_number_total             5060
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja7b11285_si_002.cif
_cod_data_source_block           delta-4
_cod_original_cell_volume        35849.5(7)
_cod_database_code               4126878
_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 0.89157(7) 0.39157(7) 0.10843(7) 0.0345(10) Uani 1 3 d S T P
Co2 Co 0.96904(11) 0.29588(11) 0.24490(11) 0.0584(10) Uani 1 1 d . . .
O2 O 0.9253(4) 0.2500 0.2500 0.021(2) Uani 1 2 d S T P
N2 N 0.9153(4) 0.3517(4) 0.1440(4) 0.031(3) Uani 1 1 d . . .
N3 N 0.9444(4) 0.3111(4) 0.1901(4) 0.037(3) Uani 1 1 d . . .
C16 C 0.9178(6) 0.3409(6) 0.1818(7) 0.051(4) Uani 1 1 d . . .
C17 C 0.9617(5) 0.3034(6) 0.1514(5) 0.042(4) Uani 1 1 d . . .
H17 H 0.9811 0.2837 0.1457 0.051 Uiso 1 1 calc R U .
C18 C 0.9454(5) 0.3296(6) 0.1240(6) 0.043(4) Uani 1 1 d . . .
P1 P 1.0000 0.5000 0.0000 0.038(3) Uani 1 12 d S T P
F1 F 0.9506(5) 0.5000 0.0000 0.057(4) Uani 1 2 d S T P
O1 O 1.0069(5) 0.2500 0.2500 0.048(4) Uani 1 2 d S T P
Co3 Co 0.88673(9) 0.38673(9) 0.38673(9) 0.0496(13) Uani 1 3 d S T P
N6 N 0.9229(5) 0.3668(5) 0.3426(5) 0.048(4) Uani 1 1 d . . .
C14 C 0.8927(7) 0.2973(7) 0.3274(7) 0.062(5) Uani 1 1 d . . .
H14A H 0.8847 0.2948 0.3552 0.094 Uiso 1 1 calc R U .
H14B H 0.9035 0.2719 0.3181 0.094 Uiso 1 1 calc R U .
H14C H 0.8696 0.3045 0.3112 0.094 Uiso 1 1 calc R U .
C12 C 0.9496(7) 0.3885(7) 0.3281(8) 0.064(6) Uani 1 1 d . . .
H12 H 0.9548 0.4150 0.3360 0.076 Uiso 1 1 calc R U .
N5 N 0.9511(4) 0.3302(4) 0.2923(4) 0.035(3) Uani 1 1 d . . .
C15 C 0.8882(6) 0.3529(6) 0.2165(6) 0.054(5) Uani 1 1 d . . .
H15A H 0.8757 0.3785 0.2101 0.081 Uiso 1 1 calc R U .
H15B H 0.9029 0.3553 0.2414 0.081 Uiso 1 1 calc R U .
H15C H 0.8676 0.3325 0.2192 0.081 Uiso 1 1 calc R U .
C13 C 0.9223(6) 0.3274(6) 0.3238(5) 0.046(4) Uani 1 1 d . . .
C11 C 0.9702(6) 0.3683(6) 0.2990(7) 0.054(5) Uani 1 1 d . . .
P2 P 0.7557(4) 0.5000 0.0000 0.083(3) Uani 1 2 d S T P
F2 F 0.7990(8) 0.5000 0.0000 0.119(10) Uani 1 2 d S T P
F4 F 0.7511(6) 0.4695(6) 0.0387(5) 0.095(5) Uani 1 1 d . . .
F3 F 0.7560(9) 0.5390(7) 0.0299(7) 0.136(9) Uani 1 1 d . . .
O3 O 0.9238(6) 0.4238(6) 0.4238(6) 0.085(9) Uani 1 3 d S T P
H3A H 0.9299 0.4482 0.4770 0.127 Uiso 0.3333 1 d R U P
H3B H 0.9734 0.4551 0.4262 0.127 Uiso 0.3333 1 d R U P
C7 C 1.0388(6) 0.3622(6) 0.1776(6) 0.046(4) Uani 1 1 d . . .
N4 N 1.0109(6) 0.3472(6) 0.2419(7) 0.070(5) Uani 1 1 d . . .
C9 C 1.0513(7) 0.3531(10) 0.2195(7) 0.072(7) Uani 1 1 d . . .
H9A H 1.0666 0.3754 0.2311 0.086 Uiso 1 1 calc R U .
H9B H 1.0676 0.3286 0.2206 0.086 Uiso 1 1 calc R U .
C6 C 1.0601(6) 0.3465(7) 0.1461(7) 0.059(5) Uani 1 1 d . . .
H6 H 1.0790 0.3264 0.1521 0.071 Uiso 1 1 calc R U .
C10 C 1.0071(6) 0.3727(5) 0.2697(5) 0.041(4) Uani 1 1 d . . .
H10 H 1.0257 0.3936 0.2729 0.049 Uiso 1 1 calc R U .
C4 C 1.0259(5) 0.3868(7) 0.0949(6) 0.051(5) Uani 1 1 d . . .
H4 H 1.0208 0.3946 0.0683 0.061 Uiso 1 1 calc R U .
C5 C 1.0562(6) 0.3580(7) 0.1051(6) 0.053(5) Uani 1 1 d . . .
H5 H 1.0731 0.3471 0.0853 0.064 Uiso 1 1 calc R U .
C3 C 1.0025(7) 0.4039(6) 0.1301(5) 0.054(5) Uani 1 1 d . . .
C8 C 1.0100(5) 0.3911(6) 0.1681(6) 0.048(4) Uani 1 1 d . . .
H8 H 0.9949 0.4023 0.1891 0.058 Uiso 1 1 calc R U .
C2 C 0.9721(7) 0.4385(6) 0.1189(6) 0.055(5) Uani 1 1 d . . .
H2A H 0.9805 0.4635 0.1318 0.066 Uiso 1 1 calc R U .
H2B H 0.9723 0.4427 0.0898 0.066 Uiso 1 1 calc R U .
N1 N 0.9329(4) 0.4288(4) 0.1314(4) 0.029(2) Uani 1 1 d . . .
C1 C 0.9166(6) 0.4525(7) 0.1625(6) 0.055(5) Uani 1 1 d . . .
H1 H 0.9318 0.4716 0.1767 0.066 Uiso 1 1 calc R U .
F5 F 0.7082(9) 0.5000 0.0000 0.143(12) Uani 1 2 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'
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'
P P 0.2955 0.4335 '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 96.3(5) . 45_556
N2 Co1 N2 96.3(5) . 20_645
N2 Co1 N2 96.3(5) 45_556 20_645
N2 Co1 N1 84.7(5) . 45_556
N2 Co1 N1 84.8(5) 45_556 45_556
N2 Co1 N1 178.4(6) 20_645 45_556
N2 Co1 N1 178.4(6) . 20_645
N2 Co1 N1 84.7(5) 45_556 20_645
N2 Co1 N1 84.8(5) 20_645 20_645
N1 Co1 N1 94.2(5) 45_556 20_645
N2 Co1 N1 84.9(5) . .
N2 Co1 N1 178.4(6) 45_556 .
N2 Co1 N1 84.7(5) 20_645 .
N1 Co1 N1 94.2(5) 45_556 .
N1 Co1 N1 94.2(5) 20_645 .
O1 Co2 N5 123.5(4) . .
O1 Co2 N3 121.1(4) . .
N5 Co2 N3 115.4(6) . .
O1 Co2 O2 82.8(5) . .
N5 Co2 O2 98.1(4) . .
N3 Co2 O2 88.6(4) . .
O1 Co2 N4 101.5(7) . .
N5 Co2 N4 77.7(7) . .
N3 Co2 N4 91.2(7) . .
O2 Co2 N4 175.2(6) . .
Co2 O2 Co2 93.1(5) . 23
C16 N2 C18 105.4(15) . .
C16 N2 Co1 142.8(13) . .
C18 N2 Co1 110.9(10) . .
C16 N3 C17 102.1(15) . .
C16 N3 Co2 128.3(13) . .
C17 N3 Co2 126.1(11) . .
N2 C16 N3 115.9(19) . .
N2 C16 C15 126.6(18) . .
N3 C16 C15 116.5(17) . .
C18 C17 N3 108.9(15) . .
C17 C18 C1 134.0(18) . 45_556
C17 C18 N2 107.4(15) . .
C1 C18 N2 118.6(17) 45_556 .
F1 P1 F1 180.0 . 10_765
F1 P1 F1 90.000(1) . 14_644
F1 P1 F1 90.000(1) 10_765 14_644
F1 P1 F1 90.000(1) . 39_554
F1 P1 F1 90.000(1) 10_765 39_554
F1 P1 F1 90.0 14_644 39_554
F1 P1 F1 90.000(1) . 17_665
F1 P1 F1 90.000(1) 10_765 17_665
F1 P1 F1 180.0 14_644 17_665
F1 P1 F1 90.0 39_554 17_665
F1 P1 F1 90.000(1) . 42_656
F1 P1 F1 90.000(1) 10_765 42_656
F1 P1 F1 90.0 14_644 42_656
F1 P1 F1 180.0 39_554 42_656
F1 P1 F1 90.0 17_665 42_656
Co2 O1 Co2 101.4(8) 23 .
N6 Co3 N6 113.2(4) 38_545 27_554
N6 Co3 N6 113.2(4) 38_545 .
N6 Co3 N6 113.2(4) 27_554 .
N6 Co3 O3 105.4(5) 38_545 .
N6 Co3 O3 105.4(5) 27_554 .
N6 Co3 O3 105.4(5) . .
C12 N6 C13 111.6(17) . .
C12 N6 Co3 121.4(15) . .
C13 N6 Co3 127.1(13) . .
N6 C12 C11 110(2) . .
C13 N5 C11 104.0(15) . .
C13 N5 Co2 136.9(12) . .
C11 N5 Co2 119.1(12) . .
C14 C13 N5 125.3(17) . .
C14 C13 N6 128.0(17) . .
N5 C13 N6 104.4(15) . .
C12 C11 N5 108.8(17) . .
C12 C11 C10 141.9(18) . .
N5 C11 C10 109.3(15) . .
F2 P2 F5 180.0 . .
F2 P2 F3 89.7(11) . .
F5 P2 F3 90.3(11) . .
F2 P2 F3 89.7(11) . 11_565
F5 P2 F3 90.3(11) . 11_565
F3 P2 F3 179(2) . 11_565
F2 P2 F4 95.3(8) . .
F5 P2 F4 84.7(8) . .
F3 P2 F4 90.8(9) . .
F3 P2 F4 89.3(9) 11_565 .
F2 P2 F4 95.3(8) . 11_565
F5 P2 F4 84.7(8) . 11_565
F3 P2 F4 89.3(9) . 11_565
F3 P2 F4 90.8(9) 11_565 11_565
F4 P2 F4 169.4(16) . 11_565
C6 C7 C8 116.4(18) . .
C6 C7 C9 119.8(19) . .
C8 C7 C9 123(2) . .
C10 N4 C9 110.8(19) . .
C10 N4 Co2 115.0(13) . .
C9 N4 Co2 131.9(17) . .
C7 C9 N4 103.6(19) . .
C7 C6 C5 125.8(19) . .
N4 C10 C11 118.1(17) . .
C5 C4 C3 115.4(17) . .
C6 C5 C4 118.1(17) . .
C8 C3 C4 120.6(18) . .
C8 C3 C2 124.5(16) . .
C4 C3 C2 114.9(17) . .
C3 C8 C7 123.6(17) . .
N1 C2 C3 111.1(15) . .
C1 N1 C2 116.3(15) . .
C1 N1 Co1 111.3(11) . .
C2 N1 Co1 131.8(13) . .
C18 C1 N1 114.5(17) 20_645 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 N2 1.928(12) .
Co1 N2 1.928(12) 45_556
Co1 N2 1.928(12) 20_645
Co1 N1 1.983(13) 45_556
Co1 N1 1.983(13) 20_645
Co1 N1 1.983(13) .
Co2 O1 1.968(11) .
Co2 N5 2.019(14) .
Co2 N3 2.043(15) .
Co2 O2 2.096(9) .
Co2 N4 2.19(2) .
O2 Co2 2.096(9) 23
N2 C16 1.30(2) .
N2 C18 1.40(2) .
N3 C16 1.35(2) .
N3 C17 1.42(2) .
C16 C15 1.55(3) .
C17 C18 1.36(3) .
C18 C1 1.38(3) 45_556
P1 F1 1.630(16) .
P1 F1 1.630(16) 10_765
P1 F1 1.630(16) 14_644
P1 F1 1.630(16) 39_554
P1 F1 1.630(16) 17_665
P1 F1 1.630(16) 42_656
O1 Co2 1.968(11) 23
Co3 N6 1.994(15) 38_545
Co3 N6 1.994(15) 27_554
Co3 N6 1.994(15) .
Co3 O3 2.12(3) .
N6 C12 1.23(3) .
N6 C13 1.44(2) .
C14 C13 1.40(3) .
C12 C11 1.35(3) .
N5 C13 1.41(2) .
N5 C11 1.42(2) .
C11 C10 1.56(3) .
P2 F2 1.43(3) .
P2 F5 1.57(3) .
P2 F3 1.62(3) .
P2 F3 1.62(3) 11_565
P2 F4 1.631(18) .
P2 F4 1.632(18) 11_565
C7 C6 1.36(3) .
C7 C8 1.38(3) .
C7 C9 1.47(3) .
N4 C10 1.25(3) .
N4 C9 1.53(3) .
C6 C5 1.41(3) .
C4 C5 1.42(3) .
C4 C3 1.50(2) .
C3 C8 1.34(3) .
C3 C2 1.56(3) .
C2 N1 1.39(2) .
N1 C1 1.40(3) .
C1 C18 1.38(3) 20_645
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 0.000 -0.002 -0.001 13335 3689 ' '
2 0.750 0.250 0.250 357 174 ' '
3 0.250 0.250 0.750 357 174 ' '
4 0.250 0.750 0.250 357 174 ' '
5 0.750 0.750 0.750 357 174 ' '
