Metal-Coordination-Induced Fusion Creates Hollow Crystalline Molecular Superstructures.
di Gregorio, Maria Chiara; Ranjan, Priyadarshi; Houben, Lothar; Shimon, Linda J. W.; Rechav, Katya; Lahav, Michal; van der Boom, Milko E.; Journal of the American Chemical Society 140 (2018) 9132–9139; doi:10.1021/jacs.8b03055

data_4132358
_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/[\s^2^(Fo^2^)+(0.1008P)^2^] where P=(Fo^2^+2Fc^2^)/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 > 2\s(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_estimated_absorpt_t_min   0.974
_shelx_estimated_absorpt_t_max   0.998
_shelxl_version_number           2013-4
_shelx_res_checksum              19578
_shelx_hkl_checksum              33081