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_4132349
_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, 0.5(C4 H8 O2)'
_chemical_formula_sum            'C50 H44 N6 O7'
_chemical_formula_weight         840.91
_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             2017-05-25
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_cell_angle_alpha                90
_cell_angle_beta                 94.083(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.7656(10)
_cell_length_b                   22.9720(15)
_cell_length_c                   23.9458(15)
_cell_measurement_reflns_used    9672
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.14
_cell_measurement_theta_min      2.25
_cell_volume                     8650.4(10)
_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    'ShelXT (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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0940
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            237374
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        23.353
_diffrn_reflns_theta_max         23.353
_diffrn_reflns_theta_min         2.196
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.088
_exptl_absorpt_correction_T_max  0.9872
_exptl_absorpt_correction_T_min  0.9800
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1325 before and 0.0650 after correction.
The Ratio of minimum to maximum transmission is 0.9927.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'light brown'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_description       irregular
_exptl_crystal_F_000             3536
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.681
_refine_diff_density_min         -0.678
_refine_diff_density_rms         0.067
_refine_ls_extinction_coef       0.00073(18)
_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   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1150
_refine_ls_number_reflns         12536
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.1114
_refine_ls_R_factor_gt           0.0813
_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^)+(0.1009P)^2^+19.4673P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2115
_refine_ls_wR_factor_ref         0.2322
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9120
_reflns_number_total             12536
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b02994_si_001.cif
_cod_data_source_block           dew412spiro7_sq
_cod_database_code               4132349
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.986
_shelx_estimated_absorpt_t_min   0.969
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C3S(H3SA,H3SB)
2.b Aromatic/amide H refined with riding coordinates:
 C5A(H5A), C6A(H6A), C12A(H12A), C13A(H13A), C15A(H15A), C17A(H17A),
 C18A(H18A), C24A(H24A), C25A(H25A), C31A(H31A), C32A(H32A), C34A(H34A),
 C36A(H36A), C37A(H37A), C40A(H40A), C41A(H41A), C42A(H42A), C43A(H43A),
 C45A(H45A), C46A(H46A), C47A(H47A), C48A(H48A), C5B(H5B), C6B(H6B), C12B(H12B),
  C13B(H13B), C15B(H15B), C17B(H17B), C18B(H18B), C24B(H24B), C25B(H25B),
 C31B(H31B), C32B(H32B), C34B(H34B), C36B(H36B), C37B(H37B), C40B(H40B),
 C41B(H41B), C42B(H42B), C43B(H43B), C45B(H45B), C46B(H46B), C47B(H47B),
 C48B(H48B)
2.c Idealised Me refined as rotating group:
 C9A(H9AA,H9AB,H9AC), C10A(H10A,H10B,H10C), C11A(H11A,H11B,H11C), C28A(H28A,
 H28B,H28C), C29A(H29A,H29B,H29C), C30A(H30A,H30B,H30C), C9B(H9BA,H9BB,H9BC),
 C10B(H10D,H10E,H10F), C11B(H11D,H11E,H11F), C28B(H28D,H28E,H28F), C29B(H29D,
 H29E,H29F), C30B(H30D,H30E,H30F), C1S(H1SA,H1SB,H1SC), C4S(H4SA,H4SB,H4SC)
;
_shelx_res_checksum              87707
_shelx_hkl_checksum              43412
_shelx_fab_checksum              99460
_olex2_submission_special_instructions 'No special instructions were received'