#------------------------------------------------------------------------------
#$Date: 2019-11-26 01:56:09 +0200 (Tue, 26 Nov 2019) $
#$Revision: 242342 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/23/4132358.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_4132358
loop_
_publ_author_name
'di Gregorio, Maria Chiara'
'Ranjan, Priyadarshi'
'Houben, Lothar'
'Shimon, Linda J. W.'
'Rechav, Katya'
'Lahav, Michal'
'van der Boom, Milko E.'
_publ_section_title
;
 Metal-Coordination-Induced Fusion Creates Hollow Crystalline Molecular
 Superstructures.
;
_journal_issue                   29
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9132
_journal_page_last               9139
_journal_paper_doi               10.1021/jacs.8b03055
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C62 H44 N4'
_chemical_formula_sum            'C62 H44 N4'
_chemical_formula_weight         845.01
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.6512(14)
_cell_length_b                   26.6512(14)
_cell_length_c                   7.0521(5)
_cell_measurement_reflns_used    1585
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.2
_cell_volume                     5009.0(5)
_computing_cell_refinement       'Rigaku CrystalClear d*trek'
_computing_data_collection       'Rigaku CrystalClear d*trek'
_computing_data_reduction        'Rigaku CrystalClear d*trek'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXT-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku XtaLAB'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1525
_diffrn_reflns_av_unetI/netI     0.0402
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            34404
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.343
_diffrn_reflns_theta_min         2.988
_diffrn_source                   'micro-focus sealed-tube'
_exptl_absorpt_coefficient_mu    0.065
_exptl_absorpt_correction_T_max  0.998
_exptl_absorpt_correction_T_min  0.997
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Rigaku CrystalClear d*trek'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.121
_exptl_crystal_description       needle
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.044
_exptl_crystal_size_min          0.038
_platon_squeeze_details
;
;
_refine_diff_density_max         0.178
_refine_diff_density_min         -0.146
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     162
_refine_ls_number_reflns         2284
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0984
_refine_ls_R_factor_gt           0.0691
_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)+(0.1008P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1680
_refine_ls_wR_factor_ref         0.1869
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1695
_reflns_number_total             2284
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja8b03055_si_002.cif
_cod_data_source_block           TPEPA
_cod_original_cell_volume        5009.0(6)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               4132358
_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.
;
_shelx_estimated_absorpt_t_min   0.974
_shelx_estimated_absorpt_t_max   0.998
_shelxl_version_number           2013-4
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'
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
C1 C 0.53254(9) 0.80782(9) 1.1270(3) 0.0384(6) Uani 1 1 d . . .
H1 H 0.5259(8) 0.8389(9) 1.204(3) 0.033(6) Uiso 1 1 d . . .
H2 H 0.4731(8) 0.7428(8) 0.797(3) 0.034(6) Uiso 1 1 d . . .
H3 H 0.5634(8) 0.8167(8) 1.044(3) 0.031(6) Uiso 1 1 d . . .
C2 C 0.48724(9) 0.79589(9) 0.9982(3) 0.0385(6) Uani 1 1 d . . .
C3 C 0.5000 0.7500 0.8765(4) 0.0384(8) Uani 1 2 d S T P
C4 C 0.47607(9) 0.83935(9) 0.8640(3) 0.0383(6) Uani 1 1 d . . .
C5 C 0.51280(9) 0.85556(9) 0.7363(3) 0.0423(6) Uani 1 1 d . . .
H5 H 0.5449 0.8421 0.7441 0.051 Uiso 1 1 calc R U .
C6 C 0.50262(10) 0.89100(10) 0.5993(3) 0.0449(6) Uani 1 1 d . . .
H6 H 0.5278 0.9008 0.5160 0.054 Uiso 1 1 calc R U .
C7 C 0.45535(10) 0.91217(9) 0.5841(3) 0.0444(6) Uani 1 1 d . . .
C8 C 0.41892(10) 0.89767(9) 0.7145(3) 0.0462(6) Uani 1 1 d . . .
H8 H 0.3872 0.9122 0.7096 0.055 Uiso 1 1 calc R U .
C9 C 0.42928(9) 0.86190(9) 0.8514(3) 0.0415(6) Uani 1 1 d . . .
H9 H 0.4043 0.8528 0.9368 0.050 Uiso 1 1 calc R U .
C10 C 0.44391(10) 0.94748(10) 0.4368(4) 0.0488(6) Uani 1 1 d . . .
C11 C 0.43298(10) 0.97579(10) 0.3120(4) 0.0505(7) Uani 1 1 d . . .
C12 C 0.41987(11) 1.00871(10) 0.1585(4) 0.0526(7) Uani 1 1 d . . .
C13 C 0.43810(13) 0.99991(11) -0.0230(4) 0.0628(8) Uani 1 1 d . . .
H13 H 0.4588 0.9725 -0.0470 0.075 Uiso 1 1 calc R U .
C14 C 0.42507(16) 1.03227(12) -0.1668(5) 0.0778(11) Uani 1 1 d . . .
H14 H 0.4377 1.0259 -0.2874 0.093 Uiso 1 1 calc R U .
N1 N 0.39585(13) 1.07185(11) -0.1447(4) 0.0818(10) Uani 1 1 d . . .
C15 C 0.37848(16) 1.08003(13) 0.0306(5) 0.0823(11) Uani 1 1 d . . .
H15 H 0.3579 1.1077 0.0507 0.099 Uiso 1 1 calc R U .
C16 C 0.38949(13) 1.04952(12) 0.1831(5) 0.0675(9) Uani 1 1 d . . .
H16 H 0.3763 1.0567 0.3022 0.081 Uiso 1 1 calc R U .
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'
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
C2 C1 C2 111.0(2) 15_567 .
C2 C1 H1 112.2(13) 15_567 .
C2 C1 H1 110.4(13) . .
C2 C1 H3 108.6(12) 15_567 .
C2 C1 H3 109.7(12) . .
H1 C1 H3 104.8(18) . .
C4 C2 C1 112.34(19) . 12_768
C4 C2 C3 107.58(18) . .
C1 C2 C3 108.10(18) 12_768 .
C4 C2 C1 111.17(19) . .
C1 C2 C1 108.84(15) 12_768 .
C3 C2 C1 108.69(17) . .
C2 C3 C2 111.9(2) 6_564 .
C2 C3 H2 110.1(14) 6_564 .
C2 C3 H2 109.4(14) . .
C9 C4 C5 117.0(2) . .
C9 C4 C2 123.0(2) . .
C5 C4 C2 119.8(2) . .
C6 C5 C4 121.7(2) . .
C6 C5 H5 119.2 . .
C4 C5 H5 119.2 . .
C5 C6 C7 120.8(2) . .
C5 C6 H6 119.6 . .
C7 C6 H6 119.6 . .
C6 C7 C8 118.1(2) . .
C6 C7 C10 121.1(2) . .
C8 C7 C10 120.8(2) . .
C9 C8 C7 120.8(2) . .
C9 C8 H8 119.6 . .
C7 C8 H8 119.6 . .
C8 C9 C4 121.5(2) . .
C8 C9 H9 119.3 . .
C4 C9 H9 119.3 . .
C11 C10 C7 177.6(3) . .
C10 C11 C12 178.5(3) . .
C16 C12 C13 117.3(3) . .
C16 C12 C11 122.3(3) . .
C13 C12 C11 120.4(3) . .
C14 C13 C12 119.0(3) . .
C14 C13 H13 120.5 . .
C12 C13 H13 120.5 . .
N1 C14 C13 124.2(3) . .
N1 C14 H14 117.9 . .
C13 C14 H14 117.9 . .
C14 N1 C15 116.3(3) . .
N1 C15 C16 123.4(3) . .
N1 C15 H15 118.3 . .
C16 C15 H15 118.3 . .
C12 C16 C15 119.7(3) . .
C12 C16 H16 120.1 . .
C15 C16 H16 120.1 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.531(3) 15_567
C1 C2 1.544(3) .
C1 H1 1.00(2) .
C1 H3 1.04(2) .
C2 C4 1.525(3) .
C2 C1 1.531(3) 12_768
C2 C3 1.532(3) .
C3 C2 1.532(3) 6_564
C3 H2 0.93(2) .
C4 C9 1.387(3) .
C4 C5 1.398(3) .
C5 C6 1.378(3) .
C5 H5 0.9300 .
C6 C7 1.384(4) .
C6 H6 0.9300 .
C7 C8 1.392(4) .
C7 C10 1.434(4) .
C8 C9 1.385(3) .
C8 H8 0.9300 .
C9 H9 0.9300 .
C10 C11 1.196(4) .
C11 C12 1.436(4) .
C12 C16 1.367(4) .
C12 C13 1.389(4) .
C13 C14 1.376(4) .
C13 H13 0.9300 .
C14 N1 1.320(5) .
C14 H14 0.9300 .
N1 C15 1.338(5) .
C15 C16 1.380(5) .
C15 H15 0.9300 .
C16 H16 0.9300 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
C2 C1 C2 C4 -176.1(2) 15_567 .
C2 C1 C2 C1 59.67(18) 15_567 12_768
C2 C1 C2 C3 -57.8(2) 15_567 .
C4 C2 C3 C2 179.1(2) . 6_564
C1 C2 C3 C2 -59.39(14) 12_768 6_564
C1 C2 C3 C2 58.59(13) . 6_564
C1 C2 C4 C9 -3.3(3) 12_768 .
C3 C2 C4 C9 115.6(2) . .
C1 C2 C4 C9 -125.5(2) . .
C1 C2 C4 C5 -178.3(2) 12_768 .
C3 C2 C4 C5 -59.5(2) . .
C1 C2 C4 C5 59.4(3) . .
C9 C4 C5 C6 -2.3(3) . .
C2 C4 C5 C6 173.0(2) . .
C4 C5 C6 C7 0.4(4) . .
C5 C6 C7 C8 1.8(4) . .
C5 C6 C7 C10 -177.3(2) . .
C6 C7 C8 C9 -2.1(4) . .
C10 C7 C8 C9 177.0(2) . .
C7 C8 C9 C4 0.1(4) . .
C5 C4 C9 C8 2.1(3) . .
C2 C4 C9 C8 -173.1(2) . .
C16 C12 C13 C14 0.2(5) . .
C11 C12 C13 C14 -179.7(3) . .
C12 C13 C14 N1 -0.1(5) . .
C13 C14 N1 C15 0.1(6) . .
C14 N1 C15 C16 -0.3(6) . .
C13 C12 C16 C15 -0.4(5) . .
C11 C12 C16 C15 179.5(3) . .
N1 C15 C16 C12 0.4(6) . .
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 0.250 -0.000 0.081 214 35 ' '
2 0.250 0.500 0.911 214 35 ' '
3 0.750 -0.000 0.411 214 35 ' '
4 0.750 0.500 0.581 214 35 ' '
