An electron-deficient metallocavitand with an unusual selectivity towards substituted benzene derivatives during co-crystallizations
Chang-Cang Huang; Jian-Jun Liu; Yong Chen; Mei-Jin Lin; Chem.Commun. 49 (2013) 11512–; doi:10.1039/c3cc46022c

data_7110098
_publ_section_title
;
 An electron-deficient metallocavitand with an unusual selectivity towards
 substituted benzene derivatives during co-crystallizations
;
_journal_name_full               Chem.Commun.
_journal_page_first              11512
_journal_paper_doi               10.1039/c3cc46022c
_journal_volume                  49
_journal_year                    2013
_chemical_formula_moiety
'C128 H96 Cl8 N24 O24 S8 Zn8, 3(C6 H5 N O2), 11.5(C4 H9 N O)'
_chemical_formula_sum            'C192 H214.5 Cl8 N38.5 O41.5 S8 Zn8'
_chemical_formula_weight         4788.56
_chemical_name_systematic
; 
 ? 
;
_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_method           SHELXL-97
_cell_angle_alpha                88.98(3)
_cell_angle_beta                 84.80(3)
_cell_angle_gamma                89.60(3)
_cell_formula_units_Z            2
_cell_length_a                   18.842(4)
_cell_length_b                   18.915(4)
_cell_length_c                   31.455(6)
_cell_measurement_reflns_used    37027
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.4971
_cell_measurement_theta_min      3.3495
_cell_volume                     11162(4)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics    'ORTEX (P.McArdle, 1995)'
_computing_publication_material  'SHELXL-97/2 (Sheldrick,1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      113(2)
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  'Saturn724+ CCD'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0646
_diffrn_reflns_av_sigmaI/netI    0.1026
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            94404
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         3.35
_exptl_absorpt_coefficient_mu    1.093
_exptl_absorpt_correction_T_max  0.8991
_exptl_absorpt_correction_T_min  0.7367
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             4944
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;
SQUEEZE removed 11.5 disordered DMA  molecules per formula unit. 
This value calculated based upon volume/count_electrons analysis.
;
_refine_diff_density_max         0.980
_refine_diff_density_min         -6.571
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2089
_refine_ls_number_reflns         49254
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      6.696
_refine_ls_R_factor_all          0.1323
_refine_ls_R_factor_gt           0.1077
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0985P)^2^+58.1695P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2739
_refine_ls_wR_factor_ref         0.2902
_reflns_number_gt                36635
_reflns_number_total             49254
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc46022c.txt
_cod_data_source_block           complex1-PhNO2(935358)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C192 H214.50 Cl8 N38.50 O41.50 S8 Zn8'
_cod_database_code               7110098