Crystal structures of the polymer precursors 3-(2,5-dimethoxy-3,4,6-trimethylphenyl)propyl methacrylate and 3-(2,4,5-trimethyl-3,6-dioxocyclohexa-1,4-dienyl)propyl methacrylate
Goswami, Shailesh K.; Hanton, Lyall R.; McAdam, C. John; Moratti, Stephen C.; Simpson, Jim; Acta Crystallographica Section E 73 (2017) 658–663; doi:10.1107/S2056989017004959

data_2242260
_publ_section_title
;
 Crystal structures of the polymer precursors
 3-(2,5-dimethoxy-3,4,6-trimethylphenyl)propyl methacrylate and
 3-(2,4,5-trimethyl-3,6-dioxocyclohexa-1,4-dienyl)propyl methacrylate
;
_journal_coeditor_code           HG5486
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              658
_journal_page_last               663
_journal_paper_doi               10.1107/S2056989017004959
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          'C16 H20 O4'
_chemical_formula_moiety         'C16 H20 O4'
_chemical_formula_sum            'C16 H20 O4'
_chemical_formula_weight         276.32
_chemical_name_systematic
;
3-(2,4,5-Trimethyl-3,6-dioxocyclohexa-1,4-dienyl)propyl methacrylate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           <i>SHELXL2014/7</i>
_cell_angle_alpha                90
_cell_angle_beta                 93.495(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   4.4096(2)
_cell_length_b                   11.8425(6)
_cell_length_c                   28.2511(16)
_cell_measurement_reflns_used    1562
_cell_measurement_temperature    89(2)
_cell_measurement_theta_max      21.11
_cell_measurement_theta_min      2.25
_cell_volume                     1472.55(13)
_computing_cell_refinement
;
APEX2 and SAINT (Bruker, 2013)
;
_computing_data_collection
;
APEX2 (Bruker, 2013)
;
_computing_data_reduction
;
SAINT (Bruker, 2013)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  2008)
;
_computing_publication_material
;
<i>SHELXL2014/7</i> (Sheldrick, 2015), enCIFer (Allen <i>et al.</i>,
2004),
PLATON (Spek, 2009),  publCIF (Westrip 2010)
;
_computing_structure_refinement
;
<i>SHELXL2014/7</i> (Sheldrick, 2015) and <i>TITAN</i>
(Hunter & Simpson, 1999)
;
_computing_structure_solution
;
SHELXS2013 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      89(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0708
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            16398
_diffrn_reflns_theta_full        24.824
_diffrn_reflns_theta_max         24.824
_diffrn_reflns_theta_min         2.889
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.785093
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2013)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular fragment'
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.130
_refine_diff_density_max         0.344
_refine_diff_density_min         -0.319
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         2509
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0772
_refine_ls_R_factor_gt           0.0491
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0609P)^2^+0.8066P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1202
_refine_ls_wR_factor_ref         0.1379
_reflns_number_gt                1774
_reflns_number_total             2509
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hg5486sup1.cif
_cod_data_source_block           II
_cod_database_code               2242260
_cod_database_fobs_code          2242260
_shelx_estimated_absorpt_t_min   0.976
_shelx_estimated_absorpt_t_max   0.989
_shelx_hkl_checksum              36214
_shelx_res_checksum              57300