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_4335036
_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            'C39 H53 N11 O4 S'
_chemical_formula_weight         771.98
_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                 91.868(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.810(4)
_cell_length_b                   15.403(5)
_cell_length_c                   18.966(6)
_cell_measurement_reflns_used    47523
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.70
_cell_volume                     4032(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1114
_diffrn_reflns_av_sigmaI/netI    0.0738
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            47523
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    0.135
_exptl_absorpt_correction_T_max  0.0226
_exptl_absorpt_correction_T_min  0.0126
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1648
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.132
_exptl_crystal_size_min          0.116
_refine_diff_density_max         0.196
_refine_diff_density_min         -0.221
_refine_diff_density_rms         0.043
_refine_ls_extinction_coef       0.00072(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     531
_refine_ls_number_reflns         7106
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.1217
_refine_ls_R_factor_gt           0.0527
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0439P)^2^+1.6893P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1007
_refine_ls_wR_factor_ref         0.1254
_reflns_number_gt                3924
_reflns_number_total             7106
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic400319b_si_002_4.cif
_cod_data_source_block           5
_cod_database_code               4335036