The syn and anti isomers of the porphyrinogen-like precursor of calix[4]phyrin: isolation, X-ray structure, anion binding and fluoride-ion-mediated proton-deuterium exchange studies.
Guchhait, Tapas; Jha, Vikesh Kumar; Mani, Ganesan; Organic & biomolecular chemistry 11 (2013) 2818–2826; doi:10.1039/c3ob40147b

data_7152896
_publ_section_title
;
 The syn and anti isomers of the porphyrinogen-like precursor of
 calix[4]phyrin: isolation, X-ray structure, anion binding and
 fluoride-ion-mediated proton-deuterium exchange studies.
;
_journal_issue                   17
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              2818
_journal_page_last               2826
_journal_paper_doi               10.1039/c3ob40147b
_journal_volume                  11
_journal_year                    2013
_chemical_formula_sum            'C38 H43.33 N6 O0.66'
_chemical_formula_weight         594.68
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
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_symmetry_space_group_name_Hall  '-P 1'
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_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                97.519(6)
_cell_angle_beta                 104.854(6)
_cell_angle_gamma                111.281(5)
_cell_formula_units_Z            3
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_cell_length_b                   13.988(3)
_cell_length_c                   17.936(3)
_cell_measurement_reflns_used    31096
_cell_measurement_temperature    295(2)
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_cell_volume                     2577.0(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker-APEX-II CCD area detector'
_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  0.0614
_diffrn_reflns_av_sigmaI/netI    0.0693
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            31096
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    0.070
_exptl_absorpt_correction_T_max  0.9944
_exptl_absorpt_correction_T_min  0.9792
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.150
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             956
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.08
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
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_refine_ls_number_reflns         9037
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_refine_ls_R_factor_all          0.1194
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0631P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1182
_refine_ls_wR_factor_ref         0.1475
_reflns_number_gt                4643
_reflns_number_total             9037
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c3ob40147b.txt
_cod_data_source_block           antiiso
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        2577.1(8)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7152896