A self-assembled M2L4 cage incorporating electron-rich 9-(1,3-dithiol-2-ylidene)fluorene units
Croué, V.; Krykun, S.; Allain, M.; Morille, Y.; Aubriet, F.; Carré, V.; Voitenko, Z.; Goeb, S.; Sallé, M.; New J. Chem. 41 (2017) 3238–; doi:10.1039/C7NJ00062F

data_7056067
_publ_section_title
;
 A self-assembled M2L4 cage incorporating electron-rich
 9-(1,3-dithiol-2-ylidene)fluorene units
;
_journal_issue                   9
_journal_name_full               'New J. Chem.'
_journal_page_first              3238
_journal_paper_doi               10.1039/C7NJ00062F
_journal_volume                  41
_journal_year                    2017
_chemical_formula_moiety         'C84 H80 N4 Pd S8, 2(B F4), 8(C2 H6 S O)'
_chemical_formula_sum            'C100 H128 B2 F8 N4 O8 Pd S16'
_chemical_formula_weight         2307.04
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-09-08T10:57:40-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2016-11-04 deposited with the CCDC.
2017-03-14 downloaded from the CCDC.
;
_cell_angle_alpha                74.016(4)
_cell_angle_beta                 67.644(4)
_cell_angle_gamma                89.049(3)
_cell_formula_units_Z            2
_cell_length_a                   17.4676(7)
_cell_length_b                   17.8158(6)
_cell_length_c                   20.0640(10)
_cell_measurement_reflns_used    6554
_cell_measurement_temperature    120.0(10)
_cell_measurement_theta_max      21.432
_cell_measurement_theta_min      3.243
_cell_volume                     5524.0(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_molecular_graphics    'DIAMOND 3.2k (Crystal Impact GbR, 2014)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 10.293
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.807
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_measurement_method       '\w and \p scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.67221
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            68110
_diffrn_reflns_theta_full        23.786
_diffrn_reflns_theta_max         32.304
_diffrn_reflns_theta_min         1.558
_exptl_absorpt_coefficient_mu    0.412
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.96692
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
        (compiled Aug 13 2014,18:06:01)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.387
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2408
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_platon_squeeze_details
;
The unit cell contains atoms not found by Fourier difference map and 
disordered dimethylsulfoxide molecules which were not modelled but the 
corresponding density was taken into account using SQUEEZE/PLATON procedure. 
The unit cell contains one void of 702 electrons/2082 A3, from which 38
electrons can be attributed to missing atoms on the alkyl chain (2 C + 7 H 
atoms not found). The others 664 electrons can be attributed to 
approxymately 16 dimethylsulfoxide molecules in the unit cell. The new 
composition was included in the calculation of the empirical formula, 
formula weight, density, linear absorption coefficient and F(000).
;
_refine_diff_density_max         1.1
_refine_diff_density_min         -1.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.708
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     969
_refine_ls_number_reflns         68110
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      0.712
_refine_ls_R_factor_all          0.2912
_refine_ls_R_factor_gt           0.0908
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1195P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2262
_refine_ls_wR_factor_ref         0.2725
_reflns_number_gt                12796
_reflns_number_total             68110
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj00062f2.cif
_cod_data_source_block           skc_twin1_hklf5_sq
_cod_depositor_comments
'Adding full bibliography for 7056066--7056067.cif.'
_cod_original_cell_volume        5524.0(4)
_cod_database_code               7056067
_platon_squeeze_void_probe_radius 1.20