Stereoselective Synthesis of Lower and Upper Rim Functionalized Tetra-α Isomers of Calix[4]pyrroles.
Díaz-Moscoso, Alejandro; Hernández-Alonso, Daniel; Escobar, Luis; Arroyave, Frank A.; Ballester, Pablo; Organic letters 19 (2017) 226–229; doi:10.1021/acs.orglett.6b03505

data_1544936
_publ_section_title
;
 Stereoselective Synthesis of Lower and Upper Rim Functionalized Tetra-\a
 Isomers of Calix[4]pyrroles.
;
_journal_issue                   1
_journal_name_full               'Organic letters'
_journal_page_first              226
_journal_page_last               229
_journal_paper_doi               10.1021/acs.orglett.6b03505
_journal_volume                  19
_journal_year                    2017
_chemical_formula_sum            'C58 H59 Cl4 N5'
_chemical_formula_weight         967.90
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_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
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 108.488(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.1993(19)
_cell_length_b                   8.9364(9)
_cell_length_c                   27.249(3)
_cell_measurement_reflns_used    6653
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.11
_cell_measurement_theta_min      2.49
_cell_volume                     4895.8(9)
_computing_cell_refinement       'Bruker APEX2 v2011.4-0'
_computing_data_collection       'Bruker APEX2 v2011.4-0'
_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 0.994
_diffrn_measured_fraction_theta_max 0.986
_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_unetI/netI     0.0956
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10188
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.388
_diffrn_reflns_theta_min         1.013
_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    0.287
_exptl_absorpt_correction_T_max  0.972
_exptl_absorpt_correction_T_min  0.471
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
 TWINABS Version 2008/0 Bruker-Nonius
 Blessing, Acta Cryst. (1995) A51 33-38
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_description       block
_exptl_crystal_F_000             2040
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.181
_refine_diff_density_min         -0.601
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     687
_refine_ls_number_reflns         10188
_refine_ls_number_restraints     153
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0978
_refine_ls_R_factor_gt           0.0859
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1013P)^2^+9.2145P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2221
_refine_ls_wR_factor_ref         0.2297
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8739
_reflns_number_total             10188
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol6b03505_si_003.cif
_cod_data_source_block           mo_cadm14-05
_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/rss-feeds/ACS/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 

 Adding full bibliography for 1544936--1544937.cif.
;
_cod_original_cell_volume        4895.8(8)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               1544936
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.894
_shelx_estimated_absorpt_t_max   0.972
_shelx_res_checksum              43844
_shelx_hkl_checksum              61091