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_1515263
_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
'C90 H66 N4 S24, Cl 1-, C16 H36 N 1+, 4 C H2 Cl2'
_chemical_formula_sum            'C110 H110 Cl9 N7 S24'
_chemical_formula_weight         2618.54
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 129.585(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   31.769(2)
_cell_length_b                   20.0818(12)
_cell_length_c                   24.852(2)
_cell_measurement_reflns_used    11369
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      26.0
_cell_measurement_theta_min      2.0
_cell_volume                     12219.2(15)
_computing_cell_refinement       'Collect software, Nonius B.V. 1998'
_computing_data_collection       'Collect software, Nonius B.V. 1998'
_computing_data_reduction
;
DENZO and Scalepack (Otwinoski and Minor, 1997)
;
_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      153(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.156
_diffrn_reflns_av_sigmaI/netI    0.3699
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            86545
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    0.666
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.922
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
DENZO and Scalepack (Otwinoski and Minor, 1997)
;
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5424
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
;
_refine_diff_density_max         0.499
_refine_diff_density_min         -0.402
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     659
_refine_ls_number_reflns         10665
_refine_ls_number_restraints     438
_refine_ls_restrained_S_all      1.154
_refine_ls_R_factor_all          0.2891
_refine_ls_R_factor_gt           0.1086
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0770P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2212
_refine_ls_wR_factor_ref         0.2479
_reflns_number_gt                3192
_reflns_number_total             10665
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2sc20636f.txt
_cod_data_source_block           calix6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_cell_volume        12219.2(14)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               1515263