The formation of a cyclic diacetal of methyl α-D-mannopyranoside with a 16-membered macrocyclic loop
Maslinska-Solich, Jolanta; Kuznik, Nikodem; Kubicki, Maciej; Kukowka, Sylwia; Chemical Communications  (2002) 984–; doi:10.1039/b202273g

data_7111212
_publ_section_title
;
 The formation of a cyclic diacetal of methyl \a-D-mannopyranoside with a
 16-membered macrocyclic loop
;
_journal_issue                   9
_journal_name_full               'Chemical Communications'
_journal_page_first              984
_journal_paper_doi               10.1039/b202273g
_journal_year                    2002
_chemical_formula_moiety         'C25 H28 O8'
_chemical_formula_sum            'C25 H28 O8'
_chemical_formula_weight         456.47
_chemical_name_systematic
; 
methyl 2,3(R):4,6(R)-di-O-[2,2-(1,4-butoxy)]phenylidene-\a-D-mannopyranoside
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 113.83(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.955(2)
_cell_length_b                   16.560(3)
_cell_length_c                   12.578(3)
_cell_measurement_reflns_used    32
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.4
_cell_measurement_theta_min      4.9
_cell_volume                     2277.8(9)
_computing_cell_refinement       'KUMA KM4 software (Kuma Diffraction, 1991)'
_computing_data_collection       'KUMA KM4 software (Kuma Diffraction, 1991)'
_computing_data_reduction        'KUMA KM4 software (Kuma Diffraction, 1991)'
_computing_molecular_graphics
;
Stereochemical Workstation (Siemens Analytical X-Ray Instruments, Inc. 1989,
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.921
_diffrn_measured_fraction_theta_max 0.921
_diffrn_measurement_device       'KM4 four-circle diffractometer'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_av_sigmaI/netI    0.0162
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3997
_diffrn_reflns_theta_full        65.92
_diffrn_reflns_theta_max         65.92
_diffrn_reflns_theta_min         3.84
_diffrn_standards_decay_%        4.17
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.825
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.324
_refine_diff_density_min         -0.167
_refine_diff_density_rms         0.042
_refine_ls_abs_structure_details 'Flack, 1983'
_refine_ls_abs_structure_Flack   0.0(2)
_refine_ls_extinction_coef       0.0012(2)
_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_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     605
_refine_ls_number_reflns         3791
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0402
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+1.0330P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0980
_refine_ls_wR_factor_ref         0.1014
_reflns_number_gt                3540
_reflns_number_total             3791
_reflns_threshold_expression     I>2\s
_cod_data_source_file            b202273gsup1.cif
_cod_data_source_block           nkx6
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 
;
_cod_original_cell_volume        2277.8(8)
_cod_original_sg_symbol_H-M      P2~1~
_cod_database_code               7111212