A chiral “Siamese-Twin” calix[4]pyrrole tetramer
Galán, Albano; Aragay, Gemma; Ballester, Pablo; Chem. Sci. 7 (2016) 5976–; doi:10.1039/C6SC01843B

data_1544044
_publ_section_title
;
 A chiral &#x201C;Siamese-Twin&#x201D; calix[4]pyrrole tetramer
;
_journal_issue                   9
_journal_name_full               'Chem. Sci.'
_journal_page_first              5976
_journal_paper_doi               10.1039/C6SC01843B
_journal_volume                  7
_journal_year                    2016
_chemical_formula_sum            'C136.5 H112 Cl4 N10 O2'
_chemical_formula_weight         2066.15
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2016-04-25 deposited with the CCDC.
2016-05-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.745(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.1450(7)
_cell_length_b                   24.8685(14)
_cell_length_c                   20.3023(12)
_cell_measurement_reflns_used    4736
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.48
_cell_measurement_theta_min      2.24
_cell_volume                     5415.8(6)
_computing_cell_refinement       'Bruker APEX2 v2014.9-0'
_computing_data_collection       'Bruker APEX2 v2014.9-0'
_computing_data_reduction        'Bruker SAINT V7.60A'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    Sir2011
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 512
_diffrn_detector_type            '4K CCD area detector APEX II'
_diffrn_measured_fraction_theta_full 0.734
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'APEX DUO Kappa 4-axis goniometer'
_diffrn_measurement_method
;
 Fullsphere data collection, phi and omega scans
;
_diffrn_measurement_specimen_support 'magnetic support with MicroMount'
_diffrn_radiation_monochromator  'Quazar MX Multilayer Optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0480
_diffrn_reflns_av_unetI/netI     0.0540
_diffrn_reflns_Laue_measured_fraction_full 0.734
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23496
_diffrn_reflns_point_group_measured_fraction_full 0.734
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         23.148
_diffrn_reflns_theta_min         1.638
_diffrn_source                   'Microfocus source E025 IuS'
_diffrn_source_current           0.6
_diffrn_source_power             50
_diffrn_source_size              '0.2 mm x 0.2 mm fine focus'
_diffrn_source_type              'Bruker APEX DUO'
_exptl_absorpt_coefficient_mu    0.170
_exptl_absorpt_correction_T_max  0.998
_exptl_absorpt_correction_T_min  0.867
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS Version 2008/1 Bruker-Nonius
 Blessing, Acta Cryst. (1995) A51 33-38
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_description       block
_exptl_crystal_F_000             2170
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.694
_refine_diff_density_min         -0.800
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     907
_refine_ls_number_reflns         6215
_refine_ls_number_restraints     525
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.1263
_refine_ls_R_factor_gt           0.0952
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1157P)^2^+22.9013P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2438
_refine_ls_wR_factor_ref         0.2659
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4674
_reflns_number_total             6215
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc01843b2.cif
_cod_data_source_block           mo_GACP055_2_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

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

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/current/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 4268 2015-11-12 08:31:59Z antanas 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_original_formula_sum        'C136.50 H112 Cl4 N10 O2'
_cod_database_code               1544044
_shelx_estimated_absorpt_t_min   0.998
_shelx_estimated_absorpt_t_max   0.998
_shelxl_version_number           2014-3
_shelx_res_checksum              61069
_shelx_hkl_checksum              30844