Dimethylcethrene: A Chiroptical Diradicaloid Photoswitch.
Ravat, Prince; Šolomek, Tomáš; Häussinger, Daniel; Blacque, Olivier; Juríček, Michal; Journal of the American Chemical Society 140 (2018) 10839–10847; doi:10.1021/jacs.8b05465

data_4132674
_publ_section_title
;
 Dimethylcethrene: A Chiroptical Diradicaloid Photoswitch.
;
_journal_issue                   34
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10839
_journal_page_last               10847
_journal_paper_doi               10.1021/jacs.8b05465
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C30 H20'
_chemical_formula_sum            'C30 H20'
_chemical_formula_weight         380.46
_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             2017-05-03
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_cell_angle_alpha                90
_cell_angle_beta                 96.824(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.82299(16)
_cell_length_b                   17.3405(4)
_cell_length_c                   13.9697(3)
_cell_measurement_reflns_used    13424
_cell_measurement_temperature    160(1)
_cell_measurement_theta_max      32.4
_cell_measurement_theta_min      2.6
_cell_volume                     1881.63(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.13a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.13a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.13a (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015b)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015a)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      160(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_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    -41.00  60.00   0.50   50.00    --  -16.19  57.00   0.00  202
  2  \w     38.00  99.00   0.50   50.00    --   15.09 178.00  90.00  122
  3  \w     38.00  99.00   0.50   50.00    --   15.09 178.00 120.00  122
  4  \w    -63.00  45.00   0.50   50.00    --   15.09 -77.00-180.00  216
  5  \w     35.00  98.00   0.50   50.00    --   15.09-178.00   0.00  126
  6  \w    -27.00  25.00   0.50   50.00    --  -16.19 -99.00 120.00  104
  7  \w    -27.00  25.00   0.50   50.00    --  -16.19 -99.00  60.00  104
  8  \w    -75.00   2.00   0.50   50.00    --  -16.19 -77.00 -90.00  154
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0320184000
_diffrn_orient_matrix_UB_12      0.0149021000
_diffrn_orient_matrix_UB_13      -0.0459249000
_diffrn_orient_matrix_UB_21      -0.0530731000
_diffrn_orient_matrix_UB_22      -0.0330135000
_diffrn_orient_matrix_UB_23      -0.0088824000
_diffrn_orient_matrix_UB_31      -0.0670762000
_diffrn_orient_matrix_UB_32      0.0190171000
_diffrn_orient_matrix_UB_33      0.0206356000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_unetI/netI     0.0204
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            29802
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.505
_diffrn_reflns_theta_min         2.349
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.076
_exptl_absorpt_correction_T_max  0.994
_exptl_absorpt_correction_T_min  0.989
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.13a (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_description       block
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.655
_refine_diff_density_min         -0.229
_refine_diff_density_rms         0.059
_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     273
_refine_ls_number_reflns         5727
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0621
_refine_ls_R_factor_gt           0.0524
_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^)+(0.0894P)^2^+0.6084P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1461
_refine_ls_wR_factor_ref         0.1530
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4777
_reflns_number_total             5727
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b05465_si_003.cif
_cod_data_source_block           juri0205
_cod_original_cell_volume        1881.62(7)
_cod_database_code               4132674
_shelx_shelxl_version_number     2016/6
_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:
 C2(H2), C3(H3), C7(H7), C8(H8), C9(H9), C11(H11), C16(H16), C17(H17),
 C18(H18), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28)
2.b Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C30(H30A,H30B,H30C)
;
_shelx_res_checksum              15226
_shelx_hkl_checksum              76910