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_4132346
_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         'C82 H56 Br2 N6 O14 Zn2'
_chemical_formula_sum            'C82 H56 Br2 N6 O14 Zn2'
_chemical_formula_weight         1639.88
_space_group_crystal_system      orthorhombic
_space_group_IT_number           47
_space_group_name_Hall           '-P 2 2'
_space_group_name_H-M_alt        'P m m m'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-08-08
_audit_creation_method
;
Olex2 1.2
(compiled 2017.07.20 svn.r3457 for OlexSys, GUI svn.r5370)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.149(2)
_cell_length_b                   15.869(3)
_cell_length_c                   22.608(5)
_cell_measurement_reflns_used    5853
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      21.79
_cell_measurement_theta_min      2.23
_cell_volume                     3999.9(14)
_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      220(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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.1317
_diffrn_reflns_av_unetI/netI     0.0577
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            23134
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        21.260
_diffrn_reflns_theta_max         21.260
_diffrn_reflns_theta_min         2.212
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.327
_exptl_absorpt_correction_T_max  0.7447
_exptl_absorpt_correction_T_min  0.5969
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1245 before and 0.0701 after correction.
The Ratio of minimum to maximum transmission is 0.8015.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.723
_exptl_crystal_description       oval
_exptl_crystal_F_000             3328
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.118
_refine_diff_density_min         -0.938
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     90
_refine_ls_number_reflns         2555
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.1089
_refine_ls_R_factor_gt           0.0697
_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^)+(0.1062P)^2^+10.4581P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1934
_refine_ls_wR_factor_ref         0.2279
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1620
_reflns_number_total             2555
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b02994_si_009.cif
_cod_data_source_block           dew4_38_1_sq
_cod_original_cell_volume        4000.1(13)
_cod_database_code               4132346
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.556
_shelx_estimated_absorpt_t_min   0.350
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 N1-C11 = C12-C11 = C13-C12 = C14-C15 = C15-C16 = C16-C17
 1.4 with sigma of 0.02
 C14-C13
 1.5 with sigma of 0.02
 C17-C17_$1
 1.5 with sigma of 0.02
3. Restrained planarity
 N1, C11, C12, C13
 with sigma of 0.1
 C14, C15, C16, C17
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: C11(0.5) H11(0.5) C12(0.5) H12(0.5) C15(0.5) C16(0.5)
6.a Riding coordinates:
 C11(H11), C12(H12)
6.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C3(H3)
;
_shelx_res_checksum              28966
_shelx_hkl_checksum              94142
_shelx_fab_checksum              7534
_olex2_submission_special_instructions 'No special instructions were received'