Synthesis of Novel Polyazacryptands for Recognition of Tetrahedral Oxoanions and Their X-ray Structures
Debasish Jana; Ganesan Mani; Carola Schulzke; Inorganic Chemistry 52 (2013) 6427–6439; doi:10.1021/ic400319b

data_4335035
_publ_contact_author_address
;Department of Chemistry
Indian Institute of Technology-Kharagpur
Kharagpur, India 721 302
;
_publ_contact_author_email       gmani@chem.iitkgp.ernet.in
_publ_contact_author_fax         91-3222-282252
_publ_contact_author_name        'Mani, Ganesan.'
_publ_contact_author_phone       91-3222-282320
_publ_section_title
;
 Synthesis of Novel Polyazacryptands for Recognition of Tetrahedral
 Oxoanions and Their X-ray Structures
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6427
_journal_page_last               6439
_journal_paper_doi               10.1021/ic400319b
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C58 H66 Cl3 N11'
_chemical_formula_weight         1023.57
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.111(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.024(3)
_cell_length_b                   15.833(3)
_cell_length_c                   23.489(5)
_cell_measurement_temperature    293(2)
_cell_volume                     5630.9(19)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker CCD APEX 2'
_diffrn_measurement_method       hemisphere
_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  0.0807
_diffrn_reflns_av_sigmaI/netI    0.0611
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            63822
_diffrn_reflns_theta_full        24.62
_diffrn_reflns_theta_max         24.62
_diffrn_reflns_theta_min         1.58
_exptl_absorpt_coefficient_mu    0.210
_exptl_absorpt_correction_T_max  0.953
_exptl_absorpt_correction_T_min  0.938
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2168
_exptl_crystal_size_max          0.303
_exptl_crystal_size_mid          0.253
_exptl_crystal_size_min          0.230
_platon_squeeze_details
;
The SQUEEZE/PLATON procedure yielded total void volume and electron 
count of 610\%A^3^ and 158 e, respectively. For Z = 4 the electron count
gives 39,5 electrons per formula. This number equals roughly one molecule of 
solvent dichloromethane per fomula. 
The fraction of solvent has been treated as a diffuse contribution 
to the overall scattering without specific atom positions.
;
_refine_diff_density_max         0.168
_refine_diff_density_min         -0.148
_refine_diff_density_rms         0.031
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.911
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     643
_refine_ls_number_reflns         9466
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.911
_refine_ls_R_factor_all          0.1135
_refine_ls_R_factor_gt           0.0580
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0926P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1435
_refine_ls_wR_factor_ref         0.1676
_reflns_number_gt                5230
_reflns_number_total             9466
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic400319b_si_002_3.cif
_cod_data_source_block           4
_cod_original_cell_volume        5631(2)
_cod_database_code               4335035