Structural and conformational studies of alcohol, diol and methyl ether derivatives of dibenzo-14-crown-4. Implications for ligand and tecton design
Olsher, Uriel; Shoham, Gil; Dalley, N. Kent; Weining, Jiang; Luboch, Elzbieta; Yu, Zong-Yuan; Knobeloch, John M.; Lee, Jong Chan; Talanov, Vladimir S.; Bartsch, Richard A.; Journal of the Chemical Society, Perkin Transactions 2  (1999) 2557–; doi:10.1039/a904180j

data_7213103
_publ_section_title
;
 Structural and conformational studies of alcohol, diol and methyl ether
 derivatives of dibenzo-14-crown-4. Implications for ligand and tecton
 design
;
_journal_issue                   11
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 2'
_journal_page_first              2557
_journal_paper_doi               10.1039/a904180j
_journal_year                    1999
_chemical_formula_sum            'C19 H22 O5'
_chemical_formula_weight         330.37
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 115.39(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.621(10)
_cell_length_b                   9.499(11)
_cell_length_c                   10.262(7)
_cell_measurement_reflns_used    14
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      10.2
_cell_measurement_theta_min      4.9
_cell_volume                     847.3(15)
_computing_cell_refinement       SAME
_computing_data_collection       'BRUKER SOFTWARE'
_computing_data_reduction        SAME
_computing_molecular_graphics    SAME
_computing_structure_refinement  'SHELXTL PC VREC. 5.03 (Sheldrick, 1994)'
_computing_structure_solution    'SHELXTL-PLUS (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'BRUKER P4'
_diffrn_measurement_method       'THETA 2THETA 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  0.1552
_diffrn_reflns_av_sigmaI/netI    0.0772
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            1270
_diffrn_reflns_theta_max         22.54
_diffrn_reflns_theta_min         2.20
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.093
_exptl_crystal_colour            COLORLESS
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_description       NEEDLE
_exptl_crystal_F_000             352
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.289
_refine_diff_density_min         -0.322
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   2.58(530)
_refine_ls_extinction_coef       0.0265(163)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.007
_refine_ls_goodness_of_fit_obs   1.156
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         1190
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_restrained_S_obs      1.156
_refine_ls_R_factor_all          0.1071
_refine_ls_R_factor_obs          0.0843
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1605P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2268
_refine_ls_wR_factor_obs         0.2071
_reflns_number_observed          821
_reflns_number_total             1190
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            904180jsup1.cif
_cod_data_source_block           COMPOUND7
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1605P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1605P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        847.3(14)
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               7213103