Crystal structure of 2,6-di-tert-butyl-4-(4-methoxybenzylidene)cyclohexa-2,5-dien-1-one, C22H28O2
Guo, Wei; Zhai, Pengda; Bai, Xiaofan; Li, Nan; Wu, Haixia; Zhang, Zhihui; He, Jingyu; Zeitschrift für Kristallographie - New Crystal Structures 237 (2022) 75–77; doi:10.1515/ncrs-2021-0394

data_8104965
_publ_section_title
;
 Crystal structure of
 2,6-di-tert-butyl-4-(4-methoxybenzylidene)cyclohexa-2,5-dien-1-one,
 C22H28O2
;
_journal_issue                   1
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              75
_journal_page_last               77
_journal_paper_doi               10.1515/ncrs-2021-0394
_journal_volume                  237
_journal_year                    2022
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C22 H28 O2'
_chemical_formula_sum            'C22 H28 O2'
_chemical_formula_weight         324.466
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_Int_Tables_number      33
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0841(9)
_cell_length_b                   16.6946(12)
_cell_length_c                   9.3837(8)
_cell_measurement_reflns_used    2545
_cell_measurement_temperature    219.99(10)
_cell_measurement_theta_max      26.4740
_cell_measurement_theta_min      2.9490
_cell_volume                     1893.1(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      219.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2684
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 0.8901
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -14.00  30.00   1.00    6.00    --  -11.27 -99.00-180.00   44
  2  \w    -87.00 -21.00   1.00    6.00    --  -11.27 -77.00  30.00   66
  3  \w    -63.00 -29.00   1.00    6.00    --   11.90 -37.00 -30.00   34
  4  \w    -53.00 -28.00   1.00    6.00    --  -11.27 106.00-166.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0456638000
_diffrn_orient_matrix_UB_12      -0.0254521000
_diffrn_orient_matrix_UB_13      0.0141152000
_diffrn_orient_matrix_UB_21      -0.0337031000
_diffrn_orient_matrix_UB_22      -0.0340038000
_diffrn_orient_matrix_UB_23      -0.0133840000
_diffrn_orient_matrix_UB_31      0.0149164000
_diffrn_orient_matrix_UB_32      0.0012685000
_diffrn_orient_matrix_UB_33      -0.0730534000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_unetI/netI     0.0526
_diffrn_reflns_Laue_measured_fraction_full 1.0000
_diffrn_reflns_Laue_measured_fraction_max 0.8901
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            8174
_diffrn_reflns_point_group_measured_fraction_full 0.8622
_diffrn_reflns_point_group_measured_fraction_max 0.7193
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         29.40
_diffrn_reflns_theta_min         2.08
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.071
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81887
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.138
_exptl_crystal_description       block
_exptl_crystal_F_000             704.314
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.1681
_refine_diff_density_min         -0.1977
_refine_diff_density_rms         0.0458
_refine_ls_abs_structure_details
'Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668.'
_refine_ls_abs_structure_Flack   -1.8(10)
_refine_ls_d_res_high            0.7238
_refine_ls_d_res_low             9.7888
_refine_ls_goodness_of_fit_ref   1.0532
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    42
_refine_ls_number_parameters     224
_refine_ls_number_reflns         3760
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.0532
_refine_ls_R_factor_all          0.0704
_refine_ls_R_factor_gt           0.0497
_refine_ls_shift/su_max          0.0002
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0414P)^2^+0.0313P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0940
_refine_ls_wR_factor_ref         0.1057
_reflns_Friedel_coverage         0.528
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              22
_reflns_limit_k_min              -22
_reflns_limit_l_max              12
_reflns_limit_l_min              -11
_reflns_number_gt                2949
_reflns_number_total             3760
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            suppl_j_ncrs-2021-0394_suppl.cif
_cod_data_source_block           TQ04
_cod_original_sg_symbol_Hall     ' P 2c -2n'
_cod_database_code               8104965
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C22(H22), C4(H4), C3(H3), C7(H7), C6(H6), C8(H8)
2.b Idealised Me refined as rotating group:
 C13(H13a,H13b,H13c), C20(H20a,H20b,H20c), C14(H14a,H14b,H14c), C21(H21a,H21b,
 H21c), C15(H15a,H15b,H15c), C19(H19a,H19b,H19c), C1(H1a,H1b,H1c)
;