Bipyrrole- and Dipyrromethane-Based Amido-imine Hybrid Macrocycles. New Receptors for Oxoanions
Evgeny A. Katayev; Nikolay V. Boev; Victor N. Khrustalev; Yuri A. Ustynyuk; I. G. Tananaev; Jonathan L. Sessler; Journal of Organic Chemistry 72 (2007) 2886–2896; doi:10.1021/jo0624849

data_4022809
_publ_section_title
;
 Bipyrrole- and Dipyrromethane-Based Amido-imine Hybrid
 Macrocycles. New Receptors for Oxoanions
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              2886
_journal_page_last               2896
_journal_paper_doi               10.1021/jo0624849
_journal_volume                  72
_journal_year                    2007
_chemical_formula_moiety         'C65 H66 N8 O2, 3(C2 H6 O S), 1.5(C H Cl3)'
_chemical_formula_sum            'C72.5 H85.5 Cl4.5 N8 O5 S3'
_chemical_formula_weight         1404.69
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                89.975(5)
_cell_angle_beta                 76.025(5)
_cell_angle_gamma                88.303(5)
_cell_formula_units_Z            2
_cell_length_a                   14.1044(19)
_cell_length_b                   14.891(2)
_cell_length_c                   18.791(3)
_cell_measurement_reflns_used    4590
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      23.5
_cell_measurement_theta_min      2.4
_cell_volume                     3828.1(10)
_computing_cell_refinement       'SAINTPlus (Bruker, 1998a)'
_computing_data_collection       'SMART (Bruker, 1998b)'
_computing_data_reduction        'SAINTPlus (Bruker, 1998a)'
_computing_molecular_graphics    'SHELXTL, v. 5.10 (Sheldrick, 1998b)'
_computing_publication_material  'SHELXTL, v. 5.10 (Sheldrick, 1998b)'
_computing_structure_refinement  'SHELXTL, v. 5.10 (Sheldrick, 1998b)'
_computing_structure_solution    'SHELXTL, v. 5.10 (Sheldrick, 1998b)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0559
_diffrn_reflns_av_sigmaI/netI    0.0991
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            33124
_diffrn_reflns_theta_full        26.06
_diffrn_reflns_theta_max         26.06
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    0.306
_exptl_absorpt_correction_T_max  0.958
_exptl_absorpt_correction_T_min  0.942
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1998a)'
_exptl_crystal_colour            light-yellow
_exptl_crystal_density_diffrn    1.219
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1482
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.069
_refine_diff_density_min         -0.913
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     946
_refine_ls_number_reflns         14790
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1858
_refine_ls_R_factor_gt           0.0973
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+16.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2073
_refine_ls_wR_factor_ref         0.2399
_reflns_number_gt                7689
_reflns_number_total             14790
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            jo0624849si20061204_055603.cif
_cod_data_source_block           DpDp-DMSO
_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 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-scan' changed
to 'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_formula_sum        'C72.50 H85.50 Cl4.50 N8 O5 S3'
_cod_database_code               4022809