N-Glycosylamines of 4,6-O-ethylidene-α-D-glucopyranose: synthesis, characterisation and structure of CO2H, Cl and F ortho-substituted phenyl derivatives and metal ion complexes of the CO2H derivative†
Sah, Ajay K.; Rao, Chebrolu P.; Saarenketo, Pauli K.; Wegelius, Elina K.; Rissanen, Kari; Kolehmainen, Erkki; Journal of the Chemical Society, Dalton Transactions  (2000) 3681–; doi:10.1039/b004854m

data_7009963
_publ_section_title
;
 N-Glycosylamines of 4,6-O-ethylidene-\a-D-glucopyranose: synthesis,
 characterisation and structure of CO2H, Cl and F ortho-substituted
 phenyl derivatives and metal ion complexes of the CO2H
 derivative&#x2020;
;
_journal_issue                   20
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3681
_journal_paper_doi               10.1039/b004854m
_journal_year                    2000
_chemical_formula_sum            'C32.5 H47 K2 N2 O17'
_chemical_formula_weight         815.92
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           5
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 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                 122.070(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.5620(10)
_cell_length_b                   13.5010(10)
_cell_length_c                   15.0410(10)
_cell_measurement_temperature    173(2)
_cell_volume                     3710.4(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1998)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1998)'
_diffrn_ambient_temperature      173(2)
_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  0.0227
_diffrn_reflns_av_sigmaI/netI    0.0537
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10452
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    0.334
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_F_000             1720
_refine_diff_density_max         0.761
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.106
_refine_ls_goodness_of_fit_obs   1.114
_refine_ls_matrix_type           full
_refine_ls_number_parameters     656
_refine_ls_number_reflns         7437
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.106
_refine_ls_restrained_S_obs      1.114
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_obs          0.0374
_refine_ls_shift/esd_max         0.006
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0514P)^2^+0.2798P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0983
_refine_ls_wR_factor_obs         0.0943
_reflns_number_observed          6796
_reflns_number_total             7437
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b004854m.txt
_cod_data_source_block           K-L(COOH)(2)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0514P)^2^+0.2798P] 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^)+(0.0514P)^2^+0.2798P] 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        3710.4(4)
_cod_original_formula_sum        'C32.50 H47 K2 N2 O17'
_cod_database_code               7009963