α-Haloketal (1'<i>R</i>,4<i>S</i>,5<i>S</i>)-dimethyl 2-(1'-bromoethyl)-2-(3,4-dimethoxyphenyl)-1,3-dioxolane-4,5-dicarboxylate
Ferri, Pedro H.; Lariucci, Carlito; Homar, Leon I. B.; Santos, Raquel F.; Maia, Elaine R.; Santos, Lourivaldo S.; Vencato, Ivo; Acta Crystallographica Section C 56 (2000) 118–120; doi:10.1107/S0108270199012962

data_2010503
_publ_section_title
;
 \a-Haloketal (1'<i>R</i>,4<i>S</i>,5<i>S</i>)-dimethyl
 2-(1'-bromoethyl)-2-(3,4-dimethoxyphenyl)-1,3-dioxolane-4,5-dicarboxylate
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              118
_journal_page_last               120
_journal_paper_doi               10.1107/S0108270199012962
_journal_volume                  56
_journal_year                    2000
_chemical_formula_moiety         'C17 H21 Br O8'
_chemical_formula_sum            'C17 H21 Br O8'
_chemical_formula_weight         433.25
_chemical_melting_point          370.5(15)
_chemical_name_systematic
;
\a-haloketal, (1'R,4S,5S)-Dimethyl 2-(1'-bromoethyl)-2-
(3",4"-dimethoxyphenyl)-1,3-dioxolane-4,5-dicarboxylate
;
_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'
_cell_angle_alpha                90.00
_cell_angle_beta                 92.23(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.728(2)
_cell_length_b                   8.414(2)
_cell_length_c                   11.674(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.96
_cell_measurement_theta_min      19.64
_cell_volume                     954.8(3)
_computing_cell_refinement
;
SET4 in CAD-4 EXPRESS
;
_computing_data_collection       'CAD-4 EXPRESS (Enraf-Nonius, 1994)'
_computing_data_reduction        'HELENA   (Spek, 1996)'
_computing_molecular_graphics
;
 ZORTEP (Zsolnai et al., 1996)
;
_computing_publication_material
;
SHELXL-97.
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device_type  'Nonius CAD-4 diffractometer'
_diffrn_measurement_method       \w--2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .018
_diffrn_reflns_av_sigmaI/netI    .053
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3275
_diffrn_reflns_theta_max         27.95
_diffrn_reflns_theta_min         2.67
_diffrn_standards_decay_%        .4
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.19
_exptl_absorpt_correction_T_max  .42
_exptl_absorpt_correction_T_min  .39
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(PLATON; Spek, 1990)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_density_meas      ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             444
_exptl_crystal_size_max          .50
_exptl_crystal_size_mid          .43
_exptl_crystal_size_min          .40
_refine_diff_density_max         .35
_refine_diff_density_min         -.31
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   -.018(11)
_refine_ls_extinction_coef       .022(2)
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   .997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         3024
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      .997
_refine_ls_R_factor_all          .0924
_refine_ls_R_factor_gt           .035
_refine_ls_shift/su_max          .001
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;
 calc w = 1/[\s^2^(Fo^2^)+(0.0352P)^2^+0.4675P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_wR_factor_ref         .086
_reflns_number_gt                1916
_reflns_number_total             3024
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bk1479.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '369-372 K' was changed to
'370.5(15)' - 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 ' 369-372 K ' was changed to
'370.5(15)' - the average value was taken and precision was
estimated.

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

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2010503
_cod_database_fobs_code          2010503