1-Ethyl 2,2-dimethyl 3-(1,3-benzodioxol-5-yl)propane-1,2,2-tricarboxylate
Hathaway, Bruce A.; Kilgore, Uriah J.; Bond, Marcus R.; Acta Crystallographica Section C 64 (2008) o456–o458; doi:10.1107/S0108270108021392

data_2016704
_publ_section_title
;
 1-Ethyl 2,2-dimethyl
 3-(1,3-benzodioxol-5-yl)propane-1,2,2-tricarboxylate
;
_journal_coeditor_code           FA3145
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o456
_journal_page_last               o458
_journal_paper_doi               10.1107/S0108270108021392
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          'C17 H20 O8'
_chemical_formula_moiety         'C17 H20 O8'
_chemical_formula_sum            'C17 H20 O8'
_chemical_formula_weight         352.33
_chemical_melting_point_gt       340
_chemical_melting_point_lt       341
_chemical_name_systematic
;
1-Ethyl 2,2-dimethyl 3-(1,3-benzodioxol-5-yl)propane-1,2,2-tricarboxylate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 109.4783(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.3799(2)
_cell_length_b                   11.7642(2)
_cell_length_c                   14.5275(3)
_cell_measurement_reflns_used    5085
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      0.998
_cell_volume                     1672.44(6)
_computing_cell_refinement       'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD software'
_computing_data_reduction
'DENZO and SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEP (Johnson, 1976)'
_computing_publication_material  'PARST (Nardelli, 1995)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution
;
maXus (Mackay <i>et al.</i>,  1999) and SIR97 (Altomare <i>et al.</i>,
1999)'
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '\k-geometry goniometer'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       CCD
_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  0.051
_diffrn_reflns_av_sigmaI/netI    0.0358
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            4861
_diffrn_reflns_theta_full        29.98
_diffrn_reflns_theta_max         29.98
_diffrn_reflns_theta_min         3.41
_exptl_absorpt_coefficient_mu    0.112
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Irregular '
_exptl_crystal_F_000             744
_exptl_crystal_size_max          .30
_exptl_crystal_size_mid          .30
_exptl_crystal_size_min          .25
_refine_diff_density_max         0.294
_refine_diff_density_min         -0.25
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     306
_refine_ls_number_reflns         4861
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_gt           0.0417
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0733P)^2^+0.1393P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0979
_refine_ls_wR_factor_ref         0.1079
_reflns_number_gt                3573
_reflns_number_total             4861
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fa3145.cif
_cod_data_source_block           I_100K
_cod_original_cell_volume        1672.49(6)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2016704
_cod_database_fobs_code          2016704