4,5-Di-tert-butyl-1,3,6,8-tetraphenyl-4,5,8a,8b-tetrahydro-as-indacene
Colon-Madera, Shakira I.; Jennings, Abby R.; Iacono, Scott T.; Balaich, Gary J.; Molbank 2023 (2023) M1663–; doi:10.3390/M1663

data_1569471
_publ_section_title
;
 4,5-Di-tert-butyl-1,3,6,8-tetraphenyl-4,5,8a,8b-tetrahydro-as-indacene
;
_journal_issue                   2
_journal_name_full               Molbank
_journal_page_first              M1663
_journal_paper_doi               10.3390/M1663
_journal_volume                  2023
_journal_year                    2023
_chemical_formula_moiety         'C44 H44'
_chemical_formula_sum            'C44 H44'
_chemical_formula_weight         572.79
_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_date             2023-04-24
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_cell_angle_alpha                90
_cell_angle_beta                 101.4620(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.66820(10)
_cell_length_b                   19.08900(10)
_cell_length_c                   25.66600(10)
_cell_measurement_reflns_used    36325
_cell_measurement_temperature    100.01(12)
_cell_measurement_theta_max      68.0910
_cell_measurement_theta_min      3.5150
_cell_volume                     6563.02(7)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(12)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_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    -73.00  26.00   0.50    1.00    --  -42.80  93.00-122.00  198
  2  \w    -13.00  73.00   0.50    1.00    --   42.80 -93.00 125.00  172
  3  \w    -81.00 -11.00   0.50    4.00    --  -80.25  93.00-122.00  140
  4  \w   -149.00 -82.00   0.50    4.00    --  -80.25 -93.00 125.00  134
  5  \w    104.00 162.00   0.50    4.00    --   93.01  93.00-122.00  116
  6  \w     24.00 106.00   0.50    4.00    --   93.01 -93.00 125.00  164
  7  \w    -28.00  26.00   0.50    1.00    --  -42.80  21.00-120.00  108
  8  \w   -108.00 -26.00   0.50    1.00    --  -42.80 -54.00 120.00  164
  9  \w    -28.00  26.00   0.50    1.00    --  -42.80  21.00   0.00  108
 10  \w   -107.00 -30.00   0.50    1.00    --  -42.80 -43.00-180.00  154
 11  \w    -28.00  26.00   0.50    1.00    --  -42.80  21.00-150.00  108
 12  \w    -30.00  24.00   0.50    1.00    --   42.80 -11.00 150.00  108
 13  \w    -22.00  37.00   0.50    1.00    --   42.80 -32.00-150.00  118
 14  \w    -30.00  24.00   0.50    1.00    --   42.80 -11.00 -30.00  108
 15  \w    -47.00 -15.00   0.50    4.00    --  -80.25  42.00  60.00   64
 16  \w    -47.00 -15.00   0.50    4.00    --  -80.25  42.00 120.00   64
 17  \w    -47.00 -15.00   0.50    4.00    --  -80.25  42.00-180.00   64
 18  \w    -47.00 -15.00   0.50    4.00    --  -80.25  42.00  30.00   64
 19  \w     44.00 127.00   0.50    4.00    --   93.01-145.00 -90.00  166
 20  \w     99.00 158.00   0.50    4.00    --   93.01 117.00-150.00  118
 21  \w     27.00  57.00   0.50    4.00    --   93.01 -50.00  30.00   60
 22  \w     28.00 109.00   0.50    4.00    --   93.01-117.00 -90.00  162
 23  \w     27.00  57.00   0.50    4.00    --   93.01 -50.00 150.00   60
 24  \w     27.00  57.00   0.50    4.00    --   93.01 -50.00   0.00   60
 25  \w     27.00  68.00   0.50    4.00    --   93.01 -59.00-180.00   82
 26  \w     27.00  68.00   0.50    4.00    --   93.01 -59.00-120.00   82
 27  \w     27.00  83.00   0.50    4.00    --   93.01 -68.00 150.00  112
 28  \w     81.00 160.00   0.50    4.00    --   93.01 145.00 -90.00  158
 29  \w     27.00  83.00   0.50    4.00    --   93.01 -68.00   0.00  112
 30  \w     27.00  57.00   0.50    4.00    --   93.01 -50.00-120.00   60
 31  \w     84.00 158.00   0.50    4.00    --   93.01  33.00  60.00  148
 32  \w     27.00  83.00   0.50    4.00    --   93.01 -68.00 -30.00  112
 33  \w    105.00 163.00   0.50    4.00    --   93.01  96.00-150.00  116
 34  \w     84.00 158.00   0.50    4.00    --   93.01  33.00-150.00  148
 35  \w     27.00  68.00   0.50    4.00    --   93.01 -59.00-150.00   82
 36  \w     27.00  68.00   0.50    4.00    --   93.01 -59.00 120.00   82
 37  \w    105.00 163.00   0.50    4.00    --   93.01  96.00 120.00  116
 38  \w     27.00  57.00   0.50    4.00    --   93.01 -50.00 -90.00   60
 39  \w     27.00  57.00   0.50    4.00    --   93.01 -50.00 120.00   60
 40  \w     27.00  83.00   0.50    4.00    --   93.01 -68.00 -60.00  112
 41  \w   -107.00 -30.00   0.50    1.00    --  -42.80 -43.00 -90.00  154
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0130309000
_diffrn_orient_matrix_UB_12      -0.0746255000
_diffrn_orient_matrix_UB_13      0.0205157000
_diffrn_orient_matrix_UB_21      -0.1070381000
_diffrn_orient_matrix_UB_22      -0.0024575000
_diffrn_orient_matrix_UB_23      -0.0332501000
_diffrn_orient_matrix_UB_31      0.0400238000
_diffrn_orient_matrix_UB_32      -0.0306048000
_diffrn_orient_matrix_UB_33      -0.0471747000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0211
_diffrn_reflns_av_unetI/netI     0.0152
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            63674
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.251
_diffrn_reflns_theta_min         2.906
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.486
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.628
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.159
_exptl_crystal_description       prism
_exptl_crystal_F_000             2464
_exptl_crystal_size_max          0.184
_exptl_crystal_size_mid          0.164
_exptl_crystal_size_min          0.055
_refine_diff_density_max         0.244
_refine_diff_density_min         -0.179
_refine_diff_density_rms         0.036
_refine_ls_extinction_coef       0.00024(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     806
_refine_ls_number_reflns         11957
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0371
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0399P)^2^+2.8060P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0904
_refine_ls_wR_factor_ref         0.0926
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10918
_reflns_number_total             11957
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            THInd1ABS.cif
_cod_data_source_block           thind1abs
_cod_database_code               1569471
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C44 H44'
_shelx_estimated_absorpt_t_max   0.974
_shelx_estimated_absorpt_t_min   0.916
_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 Ternary CH refined with riding coordinates:
 C4(H4), C5(H5), C8A(H8A), C8B(H8B), C4'(H4'), C5'(H5'), C8A'(H8A'), C8B'(H8B')
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C7(H7), C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C16(H16),
 C17(H17), C18(H18), C19(H19), C20(H20), C22(H22), C23(H23), C24(H24), C25(H25),
  C26(H26), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C2'(H2'),
 C7'(H7'), C10'(H10'), C11'(H11'), C12'(H12'), C13'(H13'), C14'(H14'),
 C16'(H16'), C17'(H17'), C18'(H18'), C19'(H19'), C20'(H20'), C22'(H22'),
 C23'(H23'), C24'(H24'), C25'(H25'), C26'(H26'), C28'(H28'), C29'(H29'),
 C30'(H30'), C31'(H31'), C32'(H32')
2.c Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C38(H38A,H38B,
 H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C34'(H34D,H34E,H34F),
 C35'(H35D,H35E,H35F), C36'(H36D,H36E,H36F), C38'(H38D,H38E,H38F), C39'(H39D,
 H39E,H39F), C40'(H40D,H40E,H40F)
;
_shelx_res_checksum              67186
_shelx_hkl_checksum              80387
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.095
_oxdiff_exptl_absorpt_empirical_full_min 0.908