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_4132338
_publ_section_title
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 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_absolute_configuration ad
_chemical_formula_moiety         '0.5(C106 H76 N4 O16 S4 Zn4)'
_chemical_formula_sum            'C53 H38 N2 O8 S2 Zn2'
_chemical_formula_weight         1025.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-12-19
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 91.054(2)
_cell_angle_gamma                90
_cell_formula_units_Z            6
_cell_length_a                   19.9556(11)
_cell_length_b                   22.8307(14)
_cell_length_c                   21.9438(12)
_cell_measurement_reflns_used    9798
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.28
_cell_volume                     9995.9(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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0709
_diffrn_reflns_av_unetI/netI     0.0627
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            153458
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.730
_diffrn_reflns_theta_max         26.730
_diffrn_reflns_theta_min         2.227
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.823
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7190
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0628 before and 0.0555 after correction.
The Ratio of minimum to maximum transmission is 0.9643.
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    1.022
_exptl_crystal_description       block
_exptl_crystal_F_000             3156
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.281
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.196(10)
_refine_ls_extinction_coef       0.00026(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     915
_refine_ls_number_reflns         21209
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0790
_refine_ls_R_factor_gt           0.0420
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0484P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0852
_refine_ls_wR_factor_ref         0.0944
_reflns_Friedel_coverage         0.950
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                14687
_reflns_number_total             21209
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b02994_si_005.cif
_cod_data_source_block           ead_3_34_1_sq
_cod_database_code               4132338
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.922
_shelx_estimated_absorpt_t_min   0.893
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.804(10)
 0.196(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C15-C14 = C12-C11 = C37-C36
 1.54 with sigma of 0.01
 C38_$1-C37 = C38-C37 = C38-C37_$1 = C38_$1-C37_$1 = C14-C13 = C13-C12
 1.54 with sigma of 0.01
 C23-C15 \\sim C8-C11 \\sim C36-C33
 with sigma of 0.01
4. Rigid bond restraints
 C33, C36, C37, C38
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
Uanis(C38) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C37) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
6. Others
 Fixed Sof: H37A(0.5) H37B(0.5) H37C(0.5) H37D(0.5) C38(0.5) H38B(0.5)
7.a Riding coordinates:
 C37(H37A,H37B,H37C,H37D), C38(H38A,H38B)
7.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B)
7.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C7(H7), C16(H16), C17(H17), C19(H19),
 C20(H20), C22(H22), C41(H41), C42(H42), C44(H44), C45(H45), C48(H48), C49(H49),
  C51(H51), C52(H52), C55(H55), C56(H56), C58(H58), C59(H59), C62(H62),
 C63(H63), C65(H65), C66(H66), C26(H26), C27(H27), C29(H29), C30(H30), C32(H32),
  C69(H69), C70(H70), C72(H72), C73(H73), C76(H76), C77(H77), C79(H79), C80(H80)
7.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C25(H25A,H25B,H25C), C35(H35A,H35B,H35C)
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_shelx_res_checksum              69202
_shelx_hkl_checksum              70219
_shelx_fab_checksum              47294
_olex2_submission_special_instructions 'No special instructions were received'