Calix[2]bispyrrolylarenes: New Expanded Calix[4]pyrroles for Fluorometric Sensing of Anions via Extended π-Conjugation.
Chandra, Brijesh; Mahanta, Sanjeev P.; Pati, Narendra N.; Baskaran, Sambath; Kanaparthi, Ravi K.; Sivasankar, Chinnappan; Panda, Pradeepta K.; Organic letters 15 (2013) 306–309; doi:10.1021/ol3032158

data_1508861
_publ_section_title
;
 Calix[2]bispyrrolylarenes: New Expanded Calix[4]pyrroles for Fluorometric
 Sensing of Anions via Extended \p-Conjugation.
;
_journal_issue                   2
_journal_name_full               'Organic letters'
_journal_page_first              306
_journal_page_last               309
_journal_paper_doi               10.1021/ol3032158
_journal_volume                  15
_journal_year                    2013
_chemical_formula_sum            'C34 H32 N4'
_chemical_formula_weight         496.64
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 91.007(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.046(3)
_cell_length_b                   18.896(4)
_cell_length_c                   21.809(6)
_cell_measurement_reflns_used    1571
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      14.75
_cell_measurement_theta_min      2.35
_cell_volume                     5375(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.3866
_diffrn_reflns_av_sigmaI/netI    0.3464
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            55270
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.43
_exptl_absorpt_coefficient_mu    0.073
_exptl_absorpt_correction_T_max  0.9956
_exptl_absorpt_correction_T_min  0.9920
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker AXS SADABS program'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.328
_refine_diff_density_min         -0.255
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     693
_refine_ls_number_reflns         10570
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.974
_refine_ls_R_factor_all          0.3897
_refine_ls_R_factor_gt           0.1356
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1516P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2981
_refine_ls_wR_factor_ref         0.4181
_reflns_number_gt                2521
_reflns_number_total             10570
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol3032158_si_001.cif
_cod_data_source_block           compound3
_cod_depositor_comments
;
The original CIF contained some information in plain text format that 
was 'glued' to  the value of '_refine_diff_density_rms' tag upon deposition.
The information was removed and stored here for further investigation. The 
following lines were extracted (delimited by #--):
IUCR check.cif alert:

RINTA01_ALERT_3_A : The value of Rint is greater than 0.25  Rint given   0.387
PLAT020_ALERT_3_A: The value of Rint is greater than 0.12 .........      0.387
PLAT026_ALERT_3_A: Ratio Observed / Unique Reflections too Low ....      24 Perc.
Authors response:
The quality of the crystal was not optimal and it was weakly diffracting. 
Although recrystallization and data collection was attempted repeatedly, 
better crystals were not obtained. This was the best one among them.
Antanas Vaitkus,
2015-03-01

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_sg_symbol_H-M      'P2(1)/c  '
_cod_database_code               1508861