Flipping the Switch: Fast Photoisomerization in a Confined Environment.
Williams, Derek E.; Martin, Corey R.; Dolgopolova, Ekaterina A.; Swifton, Anton; Godfrey, Danielle C.; Ejegbavwo, Otega A.; Pellechia, Perry J.; Smith, Mark D.; Shustova, Natalia B.; Journal of the American Chemical Society 140 (2018) 7611–7622; doi:10.1021/jacs.8b02994

data_4132350
_publ_section_title
;
 Flipping the Switch: Fast Photoisomerization in a Confined Environment.
;
_journal_issue                   24
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7611
_journal_page_last               7622
_journal_paper_doi               10.1021/jacs.8b02994
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C48 H40 N6 O6'
_chemical_formula_sum            'C48 H40 N6 O6'
_chemical_formula_weight         796.86
_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             2017-03-03
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_cell_angle_alpha                90
_cell_angle_beta                 109.466(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.2113(8)
_cell_length_b                   9.6042(4)
_cell_length_c                   25.5421(12)
_cell_measurement_reflns_used    9008
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.43
_cell_measurement_theta_min      2.42
_cell_volume                     3980.8(3)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'Bruker APEX3 v2016.5-0 (Bruker, 2016)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Bruker PHOTON-100 area detector'
_diffrn_detector_area_resol_mean 10.4
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0681
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            154012
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        26.371
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.283
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7288
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1029 before and 0.0592 after correction.
The Ratio of minimum to maximum transmission is 0.9775.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'pale green'
_exptl_crystal_colour_modifier   pale
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_description       tablet
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.269
_refine_diff_density_min         -0.258
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     587
_refine_ls_number_reflns         8112
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0634
_refine_ls_R_factor_gt           0.0451
_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^)+(0.0419P)^2^+2.3907P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0952
_refine_ls_wR_factor_ref         0.1030
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6449
_reflns_number_total             8112
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b02994_si_002.cif
_cod_data_source_block           spiro77
_cod_database_code               4132350
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.995
_shelx_estimated_absorpt_t_min   0.981
_olex2_refinement_description
;
1.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C12(H12), C13(H13), C15(H15), C17(H17), C18(H18), C24(H24),
 C25(H25), C31(H31), C32(H32), C34(H34), C36(H36), C37(H37), C40(H40), C41(H41),
  C42(H42), C43(H43), C45(H45), C46(H46), C47(H47), C48(H48)
1.b Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C28(H28A,H28B,
 H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C)
;
_shelx_res_checksum              41411
_shelx_hkl_checksum              36768
_olex2_submission_special_instructions 'No special instructions were received'