Stable core-modified calixsmaragdyrins: synthesis, structure and specific sensing of the hydrogen sulfate ion.
Chatterjee, Tamal; Ghosh, Avijit; Madhu, Sheri; Ravikanth, Mangalampalli; Dalton transactions (Cambridge, England : 2003) 43 (2014) 6050–6058; doi:10.1039/c3dt53134a

data_7029524
_publ_section_title
;
 Stable core-modified calixsmaragdyrins: synthesis, structure and specific
 sensing of the hydrogen sulfate ion.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6050
_journal_page_last               6058
_journal_paper_doi               10.1039/c3dt53134a
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C37 H28 N4 O, H2 O'
_chemical_formula_sum            'C37 H30 N4 O2'
_chemical_formula_weight         562.65
_chemical_name_common            TC1'
_space_group_IT_number           86
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4bc'
_symmetry_space_group_name_H-M   'P 42/n :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   23.5396(4)
_cell_length_b                   23.5396(4)
_cell_length_c                   9.9876(2)
_cell_measurement_reflns_used    20826
_cell_measurement_temperature    100.4(2)
_cell_measurement_theta_max      30.7970
_cell_measurement_theta_min      2.2106
_cell_volume                     5534.26(17)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_molecular_graphics
;
 ORTEP3 for Windows (L. J. Farrugia, J. Appl. Crystallogr. 1997, 30, 565.)
;
_computing_publication_material
;
WinGX v1.80.05 (L. J. Farrugia, J. Appl. Cryst., 1999, 32, 837-838.)
;
_computing_structure_refinement
;
 SHELXL-97 (G. M. Sheldrick, Acta Cryst. (2008). A64, 112-122)
;
_computing_structure_solution
;
 SIR-92 (A. Altomare, G. Cascarano, C. Giacovazzo and A. Guagliardi,
 J. Appl. Crystallogr. 1993, 26, 343-350.)
;
_diffrn_ambient_temperature      100.4(2)
_diffrn_detector_area_resol_mean 16.1419
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0492
_diffrn_reflns_av_sigmaI/netI    0.0206
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            122109
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         2.22
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95732
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2368
_exptl_crystal_recrystallization_method
;
 From solution in methylenechloride at 20 deg C
;
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.421
_refine_diff_density_min         -0.555
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     404
_refine_ls_number_reflns         7352
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0494
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0528P)^2^+3.9085P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1170
_refine_ls_wR_factor_ref         0.1233
_reflns_number_gt                6245
_reflns_number_total             7352
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c3dt53134a.txt
_cod_data_source_block           rm2bw
_cod_original_sg_symbol_H-M      P42/n
_cod_original_formula_sum        'C37 H30 N4 O2 '
_cod_database_code               7029524