Methyl 3,3,6,6-tetramethyl-1,8-dioxo-4,5,7,9-tetrahydro-2<i>H</i>-xanthene-9-carboxylate
Detert, Heiner; Kluge, Laura; Schollmeyer, Dieter; IUCrData 5 (2020) x201018–; doi:10.1107/S2414314620010184

data_1558687
_publ_section_title
;
 Methyl
 3,3,6,6-tetramethyl-1,8-dioxo-4,5,7,9-tetrahydro-2<i>H</i>-xanthene-9-carboxylate
;
_journal_coeditor_code           GG4005
_journal_issue                   7
_journal_name_full               IUCrData
_journal_page_first              x201018
_journal_paper_doi               10.1107/S2414314620010184
_journal_volume                  5
_journal_year                    2020
_chemical_formula_iupac          'C19 H24 O5'
_chemical_formula_moiety         'C19 H24 O5'
_chemical_formula_sum            'C19 H24 O5'
_chemical_formula_weight         332.38
_chemical_name_systematic
'Methyl 3,3,6,6-tetramethyl-1,8-dioxo-4,5,7,9-tetrahydro-2<i>H</i>-xanthene-9-carboxylate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 113.295(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1494(10)
_cell_length_b                   9.6899(6)
_cell_length_c                   14.8185(13)
_cell_measurement_reflns_used    9146
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.22
_cell_measurement_theta_min      2.58
_cell_volume                     1734.2(2)
_computing_cell_refinement
;
<i>X-AREA Recipe</i> (Stoe & Cie, 2019)
;
_computing_data_collection
;
<i>X-AREA WinXpose</i> (Stoe & Cie, 2019)
;
_computing_data_reduction
;
<i>X-AREA Integrate</i> (Stoe & Cie, 2019)
;
_computing_molecular_graphics
;
PLATON (Spek, 2020)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015)
;
_computing_structure_solution
;
SIR-2004 (Burla <i>et al.</i>,  2005)
;
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_unetI/netI     0.0457
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            8583
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.949
_diffrn_reflns_theta_min         2.580
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_exptl_absorpt_coefficient_mu    0.091
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.273
_exptl_crystal_description       plate
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.242
_refine_diff_density_min         -0.300
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     222
_refine_ls_number_reflns         4123
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.1134
_refine_ls_R_factor_gt           0.0719
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0577P)^2^+2.4014P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1551
_refine_ls_wR_factor_ref         0.1845
_reflns_number_gt                2784
_reflns_number_total             4123
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            gg4005sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1558687
_cod_database_fobs_code          1558687
_shelx_estimated_absorpt_t_min   0.980
_shelx_estimated_absorpt_t_max   0.995
_shelx_hkl_checksum              93000
_shelx_res_checksum              64878