Photochromic Reaction by Red Light via Triplet Fusion Upconversion.
Tokunaga, Ayako; Uriarte, Lucas Martinez; Mutoh, Katsuya; Fron, Eduard; Hofkens, Johan; Sliwa, Michel; Abe, Jiro; Journal of the American Chemical Society  (2019) –; doi:10.1021/jacs.9b08219

data_4127316
_publ_section_title
;
 Photochromic Reaction by Red Light via Triplet Fusion Upconversion.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b08219
_journal_year                    2019
_chemical_formula_moiety         'C49 H40 N2 O'
_chemical_formula_sum            'C49 H40 N2 O'
_chemical_formula_weight         672.83
_chemical_name_systematic        Pery-RPIC
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2019-08-07
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_cell_angle_alpha                101.242(4)
_cell_angle_beta                 92.464(4)
_cell_angle_gamma                110.000(4)
_cell_formula_units_Z            2
_cell_length_a                   11.9427(6)
_cell_length_b                   12.7996(6)
_cell_length_c                   12.8505(6)
_cell_measurement_reflns_used    11152
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.4280
_cell_measurement_theta_min      1.9310
_cell_volume                     1797.60(16)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.935
_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     52.00  95.00   0.50   40.00    --   20.00  54.00  52.14   86
  2  \w    -72.00 -27.00   0.50   40.00    --   20.00  54.00  78.80   90
  3  \w     40.00 107.00   0.50   40.00    --   20.00  54.00  78.80  134
  4  \w    -73.00 108.00   0.50   40.00    --   20.00  54.00 -83.82  362
  5  \w    -74.00 108.00   0.50   40.00    --   20.00  54.00 150.00  364
  6  \w      1.00  44.00   0.50   40.00    --   20.00  54.00-180.00   86
  7  \w    -68.00  59.00   0.50   40.00    --   20.00  54.00-120.00  254
  8  \w    -71.00 -42.00   0.50   40.00    --   20.00  54.00 120.00   58
  9  \w     20.00  45.00   0.50   40.00    --   20.00  54.00 120.00   50
 10  \w     72.00  97.00   0.50   40.00    --   20.00  54.00 120.00   50
 11  \w     75.00 100.00   0.50   40.00    --   20.00  54.00 -60.00   50
 12  \w    -68.00  61.00   0.50   40.00    --   20.00  54.00-150.00  258
 13  \w    -74.00 -49.00   0.50   40.00    --   20.00  54.00  30.00   50
 14  \w    -67.00   2.00   0.50   40.00    --   20.00  54.00 -30.00  138
 15  \w     19.00  44.00   0.50   40.00    --   20.00  54.00  52.14   50
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II (JP)'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0427665000
_diffrn_orient_matrix_UB_12      -0.0078274000
_diffrn_orient_matrix_UB_13      0.0371265000
_diffrn_orient_matrix_UB_21      -0.0324313000
_diffrn_orient_matrix_UB_22      0.0252739000
_diffrn_orient_matrix_UB_23      -0.0279870000
_diffrn_orient_matrix_UB_31      -0.0342242000
_diffrn_orient_matrix_UB_32      -0.0544084000
_diffrn_orient_matrix_UB_33      -0.0324164000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_av_unetI/netI     0.0528
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.935
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            33685
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.935
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.694
_diffrn_reflns_theta_min         2.098
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.073
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93512
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53a (Rigaku Oxford Diffraction, 2019)
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    1.243
_exptl_crystal_description       block
_exptl_crystal_F_000             712
_exptl_crystal_preparation       synthesized
_exptl_crystal_recrystallization_method 'recrestalized in acetonitrile'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.440
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     629
_refine_ls_number_reflns         10437
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.971
_refine_ls_R_factor_all          0.0803
_refine_ls_R_factor_gt           0.0538
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1372
_refine_ls_wR_factor_ref         0.1515
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7774
_reflns_number_total             10437
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b08219_si_002.cif
_cod_data_source_block           20190722_peryrpic
_cod_database_code               4127316
_shelx_shelxl_version_number     2018/3
_publ_section_exptl
;
Any special experimental details
;
_chemical_oxdiff_formula         C49H40N2O
_chemical_oxdiff_usercomment     acetonitrile
_shelx_estimated_absorpt_t_max   0.993
_shelx_estimated_absorpt_t_min   0.985
_diffrn_oxdiff_digest_frames
;
0192fed031757fe43dbce590a6906e678e0208069a2
;
_diffrn_oxdiff_digest_hkl
;
011511eb3914659d787c4a1322795312844a63
;
_reflns_odcompleteness_completeness 99.18
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
;
_shelx_res_checksum              68823
_shelx_hkl_checksum              13352
_olex2_date_sample_data_collection 2019-07-23
_olex2_date_sample_submission    2019-07-22
_olex2_exptl_crystal_mounting_method 'loop and Parabar 10312'
_olex2_submission_original_sample_id Pery-RPIC
_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 1.159
_oxdiff_exptl_absorpt_empirical_full_min 0.914