Study of a diastereoisomeric dihydrothiophene derivative at 150K
María Jesús Diánez; María Dolores Estrada; Amparo López-Castro; Simeón Pérez-Garrido; Acta Crystallographica Section C 55 (1999) 1020–1023; doi:10.1107/S010827019900102X

data_2008586
_publ_section_title
;
 Study of a diastereoisomeric dihydrothiophene derivative at 150K
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1020
_journal_page_last               1023
_journal_paper_doi               10.1107/S010827019900102X
_journal_volume                  55
_journal_year                    1999
_chemical_formula_moiety         'C41 H45 N3 O14 S'
_chemical_formula_sum            'C41 H45 N3 O14 S'
_chemical_formula_weight         835.88
_chemical_melting_point          465.0(10)
_chemical_name_systematic
1-(2R,3R)-5-(N-benzyl-N-methylamino)-2-[N-(4-methoxyphenyl)carbamoyl]-4-nitro-2-phenyl-2,3-dihydro-3-thienyl]-1,2,3,4,5-penta-O-acetyl-D-manno-pentitol
_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           PARSTCIF
_cell_angle_alpha                90.00
_cell_angle_beta                 96.100(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2.00
_cell_length_a                   15.670(4)
_cell_length_b                   10.556(2)
_cell_length_c                   12.258(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    150.0(10)
_cell_measurement_theta_max      11
_cell_measurement_theta_min      5
_cell_volume                     2016.1(9)
_computing_cell_refinement
'SET4 (de Boer & Duisenberg, 1984) and CELDIM in CAD-4 Software'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        'XRAY76 System (Stewart et al., 1976)'
_computing_molecular_graphics    'PLATON94 (Spek, 1994)'
_computing_publication_material
'PARST (Nardelli, 1983b) and PARSTCIF (Nardelli, 1991)'
_computing_structure_refinement  'XRAY76 System'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150.0(10)
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.000
_diffrn_reflns_av_sigmaI/netI    0.023
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6093
_diffrn_reflns_theta_max         29.83
_diffrn_reflns_theta_min         2.01
_diffrn_standards_decay_%        none
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.153
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.3769
_exptl_crystal_description       Prism
_exptl_crystal_F_000             880.0
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.744
_refine_diff_density_min         -0.412
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   -0.01(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.047
_refine_ls_goodness_of_fit_obs   1.054
_refine_ls_hydrogen_treatment    'not refined'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     712
_refine_ls_number_reflns         6093
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.047
_refine_ls_restrained_S_obs      1.054
_refine_ls_R_factor_all          0.047
_refine_ls_R_factor_obs          .042
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0983P)^2^+0.0069P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.124
_refine_ls_wR_factor_obs         .119
_reflns_number_observed          5603
_reflns_number_total             6093
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            na1392.cif
_cod_data_source_block           M3F
_cod_depositor_comments
;
 Changing the _atom_site_occupancy data item value from '.' to '1'
 for all fully occupied atom sites.

 Antanas Vaitkus,
 2017-02-10

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 

The following automatic conversions were performed:

'_chemical_melting_point' value '464-466K' was changed to '465.0(10)'
- the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_chemical_melting_point' value '464-466K' was changed to '465.0(10)'
- the average value was taken and precision was
estimated.

'_geom_hbond_publ_flag' value 'Y' changed to 'y'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (8
times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0983P)^2^+0.0069P] 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^)+(0.0983P)^2^+0.0069P] 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        2016.2(9)
_cod_original_sg_symbol_Hall     'P 2y1'
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_sum        'C41 H45 N3 O14 S1'
_cod_database_code               2008586