Isomeric 2,6-Pyridino-Cryptands Based on Dibenzo-24-crown-8
Harry W. Gibson; Hong Wang; Carla Slebodnick; Joseph Merola; W. Scott Kassel; Arnold L. Rheingold; Journal of Organic Chemistry 72 (2007) 3381–3393; doi:10.1021/jo070030l

data_4022872
_publ_contact_author_address
;Department of Chemistry (0212)
Virginia Tech
Blacksburg, VA 24061
;
_publ_contact_author_email       hwgibson@vt.edu
_publ_contact_author_fax         540-231-8517
_publ_contact_author_name        'Gibson, Harry W.'
_publ_contact_author_phone       540-231-5902
_publ_section_title
;
 Isomeric 2,6-Pyridino-Cryptands Based on Dibenzo-24-crown-8
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              3381
_journal_page_last               3393
_journal_paper_doi               10.1021/jo070030l
_journal_volume                  72
_journal_year                    2007
_chemical_formula_moiety         'C33 H37 N O12, C14 H18 N2 O2, 2(F6 P)'
_chemical_formula_sum            'C47 H55 F12 N3 O14 P2'
_chemical_formula_weight         1175.88
_chemical_name_common            cs537
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                80.93(2)
_cell_angle_beta                 75.01(3)
_cell_angle_gamma                71.65(2)
_cell_formula_units_Z            2
_cell_length_a                   10.545(3)
_cell_length_b                   13.057(3)
_cell_length_c                   19.973(6)
_cell_measurement_reflns_used    1332
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      55.0
_cell_measurement_theta_min      2.3
_cell_volume                     2512.7(12)
_computing_cell_refinement       'CrysAlis (Oxford Diffraction)'
_computing_data_collection       'CrysAlis (Oxford Diffraction)'
_computing_data_reduction        'CrysAlis (Oxford Diffraction)'
_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      100(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 4.1570
_diffrn_detector_type            'Oxford Diffraction Onyx CCD'
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction PX Ultra'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_sigmaI/netI    0.0554
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            11884
_diffrn_reflns_theta_full        66.60
_diffrn_reflns_theta_max         66.60
_diffrn_reflns_theta_min         4.09
_diffrn_source                   'Enhance (Cu) X-ray Source'
_diffrn_source_current           40
_diffrn_source_voltage           50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.813
_exptl_absorpt_correction_T_max  0.929
_exptl_absorpt_correction_T_min  0.834
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'CrysAlis (Oxford Diffraction)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'triangular plate'
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.129
_exptl_crystal_size_mid          0.129
_exptl_crystal_size_min          0.045
_refine_diff_density_max         0.759
_refine_diff_density_min         -0.348
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     788
_refine_ls_number_reflns         8778
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0956
_refine_ls_R_factor_gt           0.0683
_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^)+(0.0763P)^2^+5.3725P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1708
_refine_ls_wR_factor_ref         0.1841
_reflns_number_gt                6310
_reflns_number_total             8778
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo070030lrom20070106_120115.cif
_cod_data_source_block           4.6
_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.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4022872