Regioselective routes to disubstituted dibenzo crown ethers and their complexations.
Gibson, Harry W.; Wang, Hong; Bonrad, Klaus; Jones, Jason W.; Slebodnick, Carla; Zackharov, Lev N.; Rheingold, Arnold L.; Habenicht, Bradley; Lobue, Peter; Ratliff, Amy E.; Organic & biomolecular chemistry 3 (2005) 2114–2121; doi:10.1039/b503072m

data_7150072
_publ_section_title
;
 Regioselective routes to disubstituted dibenzo crown ethers and their
 complexations.
;
_journal_issue                   11
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              2114
_journal_page_last               2121
_journal_paper_doi               10.1039/b503072m
_journal_volume                  3
_journal_year                    2005
_chemical_formula_moiety
'C28 H36 O12, C14 H16 N, P F6, C0.265 H1.060 O0.265'
_chemical_formula_sum            'C42.26 H53.06 F6 N O12.27 P'
_chemical_formula_weight         916.31
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 97.20(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.324(6)
_cell_length_b                   22.806(6)
_cell_length_c                   26.470(8)
_cell_measurement_reflns_used    967
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      18.97
_cell_measurement_theta_min      2.43
_cell_volume                     8579(5)
_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_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur2'
_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  0.0570
_diffrn_reflns_av_sigmaI/netI    0.0770
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            32751
_diffrn_reflns_theta_full        30.07
_diffrn_reflns_theta_max         30.07
_diffrn_reflns_theta_min         2.73
_diffrn_standards_decay_%        <2%
_diffrn_standards_interval_count 50
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.154
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3846
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.084
_exptl_crystal_size_min          0.028
_refine_diff_density_max         0.909
_refine_diff_density_min         -0.723
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.962
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     571
_refine_ls_number_reflns         12526
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.962
_refine_ls_R_factor_all          0.1119
_refine_ls_R_factor_gt           0.0578
_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^)+(0.1061P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1477
_refine_ls_wR_factor_ref         0.1901
_reflns_number_gt                7038
_reflns_number_total             12526
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b503072m.txt
_cod_data_source_block           cs539
_cod_depositor_comments
;
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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7150072