Synthesis and recognition properties of higher order tetrathiafulvalene (TTF) calix[n]pyrroles (n = 4‒6)
Park, Jung Su; Bejger, Christopher; Larsen, Karina R.; Nielsen, Kent A.; Jana, Atanu; Lynch, Vincent M.; Jeppesen, Jan O.; Kim, Dongho; Sessler, Jonathan L.; Chemical Science 3 (2012) 2685–; doi:10.1039/c2sc20636f

data_1515264
_publ_section_title
;
 Synthesis and recognition properties of higher order tetrathiafulvalene
 (TTF) calix[n]pyrroles (n = 4--6)
;
_journal_issue                   9
_journal_name_full               'Chemical Science'
_journal_page_first              2685
_journal_paper_doi               10.1039/c2sc20636f
_journal_volume                  3
_journal_year                    2012
_chemical_formula_moiety
'C75 H55 N5 S20, C24 H52 N 1+, Cl 1-, 2 C5 H12, C H2 Cl2'
_chemical_formula_sum            'C110 H127 Cl3 N6 S20'
_chemical_formula_weight         2280.73
_chemical_name_systematic
;
?
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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            4
_cell_length_a                   28.3045(9)
_cell_length_b                   24.6469(8)
_cell_length_c                   17.5652(6)
_cell_measurement_temperature    93(2)
_cell_volume                     12253.8(7)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
_computing_structure_refinement  'XL SHELXTL/PC, Siemens Analytical'
_computing_structure_solution
;

SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C.,
Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R.
;
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 0.886
_diffrn_measured_fraction_theta_max 0.886
_diffrn_measurement_device_type  'Rigaku R-Axis Spider with Image Plate'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0710
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10554
_diffrn_reflns_theta_full        70.00
_diffrn_reflns_theta_max         70.00
_diffrn_reflns_theta_min         6.72
_exptl_absorpt_coefficient_mu    4.215
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4800
_refine_diff_density_max         0.755
_refine_diff_density_min         -0.555
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.651
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     774
_refine_ls_number_reflns         10554
_refine_ls_number_restraints     1021
_refine_ls_restrained_S_all      1.630
_refine_ls_R_factor_all          0.1520
_refine_ls_R_factor_gt           0.0874
_refine_ls_shift/su_max          0.032
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0789P)^2^+1.9557P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2161
_refine_ls_wR_factor_ref         0.2662
_reflns_number_gt                5599
_reflns_number_total             10554
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2sc20636f.txt
_cod_data_source_block           js417
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               1515264