The 2:1 Adduct of an α-<small>L</small>-Altropyranose Derivative with Hexafluoro-2,6-dihydroxy-2,6-bis(trifluoromethyl)-4-heptanone at 173 K
Kopf, J.; Sheldrick, G.; Reinke, H.; Rentsch, D.; Miethchen, R.; Acta Crystallographica Section C 51 (1995) 1198–1201; doi:10.1107/S0108270194011157

data_2003602
_publ_section_title
;
 The 2:1 Adduct of an \a-<small>L</small>-Altropyranose Derivative with
 Hexafluoro-2,6-dihydroxy-2,6-bis(trifluoromethyl)-4-heptanone at 173 K
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1198
_journal_page_last               1201
_journal_paper_doi               10.1107/S0108270194011157
_journal_volume                  51
_journal_year                    1995
_chemical_formula_sum            'C43 H52 F24 N2 O15'
_chemical_formula_weight         1292.87
_chemical_melting_point          374.5(5)
_chemical_name_systematic
;
Methyl 2-O-(Cyclohexylcarbamoyl)-6-deoxy-3,4-O-
-(hexafluoroisopropylidene)-\a-L-altropyranoside
;
_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'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.0
_cell_angle_beta                 116.47(1)
_cell_angle_gamma                90.0
_cell_formula_units_Z            2
_cell_length_a                   11.623(1)
_cell_length_b                   20.861(2)
_cell_length_c                   12.570(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(1)
_cell_measurement_theta_max      50.9
_cell_measurement_theta_min      42.0
_cell_volume                     2728.3(5)
_computing_cell_refinement       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        'CADSHEL (Kopf, 1987)'
_computing_molecular_graphics    'SHELXTL-Plus (Sheldrick, 1992)'
_computing_publication_material
'CIF2TEX (Kopf, 1992a) and FCF2FOC (Kopf, 1992b)'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1994)'
_computing_structure_solution    'SHELXS90 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173.0(10)
_diffrn_measurement_device       'Enraf-Nonius CAD-4 diffractometer'
_diffrn_measurement_method       '2\q/\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_sigmaI/netI    0.0230
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12030
_diffrn_reflns_theta_max         76.5
_diffrn_reflns_theta_min         3.5
_diffrn_standards_decay_%        1
_diffrn_standards_interval_time  '120 min'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.522
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.574
_exptl_crystal_description       'transparent prisms'
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.386
_refine_diff_density_min         -0.243
_refine_ls_abs_structure_details '\c = 0.12(8) (Flack, 1983)'
_refine_ls_abs_structure_Flack   0.12(8)
_refine_ls_extinction_coef       0.0013(2)
_refine_ls_extinction_method     SHELXL93
_refine_ls_goodness_of_fit_all   1.038
_refine_ls_goodness_of_fit_obs   1.028
_refine_ls_hydrogen_treatment    'H atoms with riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     816
_refine_ls_number_reflns         11027
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.044
_refine_ls_restrained_S_obs      1.028
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_obs          0.0475
_refine_ls_shift/esd_max         0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;
calc w = 1/[\s^2^(F~o~^2^) + (0.0886P)^2^ + 0.9226P]
where P = (F~o~^2^ + 2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.1284
_refine_ls_wR_factor_obs         0.1246
_reflns_number_observed          10719
_reflns_number_total             11034
_reflns_observed_criterion       I>2sigma(I)
_cod_data_source_file            se1073.cif
_cod_data_source_block           ren35
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '374-375 K' was changed to '374.5(5)'
- the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        2728.3(4)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2003602