Connecting Wires: Photoinduced Electronic Structure Modulation in Metal-Organic Frameworks.
Dolgopolova, Ekaterina A.; Galitskiy, Vladimir A.; Martin, Corey R.; Gregory, Haley N.; Yarbrough, Brandon J.; Rice, Allison M.; Berseneva, Anna A.; Ejegbavwo, Otega A.; Stephenson, Kenneth S.; Kittikhunnatham, Preecha; Karakalos, Stavros G.; Smith, Mark D.; Greytak, Andrew B.; Garashchuk, Sophya; Shustova, Natalia B.; Journal of the American Chemical Society 141 (2019) 5350–5358; doi:10.1021/jacs.8b13853

data_4128382
_publ_section_title
;
 Connecting Wires: Photoinduced Electronic Structure Modulation in
 Metal-Organic Frameworks.
;
_journal_issue                   13
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5350
_journal_page_last               5358
_journal_paper_doi               10.1021/jacs.8b13853
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         '0.5(C114 H84 N4 O16 S4 Zn4)'
_chemical_formula_sum            'C57 H42 N2 O8 S2 Zn2'
_chemical_formula_weight         1077.78
_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             2018-01-10
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-12-02 deposited with the CCDC.
2018-12-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.562(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   26.4692(19)
_cell_length_b                   17.4806(13)
_cell_length_c                   29.688(2)
_cell_measurement_reflns_used    9272
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.20
_cell_measurement_theta_min      2.38
_cell_volume                     13353.5(17)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.1400
_diffrn_reflns_av_unetI/netI     0.0679
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            263812
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        23.430
_diffrn_reflns_theta_max         23.431
_diffrn_reflns_theta_min         2.193
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.825
_exptl_absorpt_correction_T_max  0.8619
_exptl_absorpt_correction_T_min  0.8094
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0785 before and 0.0622 after correction.
The Ratio of minimum to maximum transmission is 0.9391.
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    1.072
_exptl_crystal_description       irregular
_exptl_crystal_F_000             4432
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.093
_refine_diff_density_min         -0.767
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1325
_refine_ls_number_reflns         19451
_refine_ls_number_restraints     559
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.1305
_refine_ls_R_factor_gt           0.0866
_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^)+(0.0729P)^2^+119.1946P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2067
_refine_ls_wR_factor_ref         0.2308
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12395
_reflns_number_total             19451
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b13853_si_002.cif
_cod_data_source_block           ead3_34_4_sq
_cod_database_code               4128382
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.937
_shelx_estimated_absorpt_t_min   0.852
_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. Shared sites
{O13A, O13B}
{O14A, O14B}
{O15A, O15B}
{O16A, O16B}
{C99, C199}
{C108, C208}
3. Restrained planarity
 C99, C100, C105, C104, C103, C102, C101
 with sigma of 0.01
 C108, C109, C110, C111, C112, C113, C114
 with sigma of 0.01
 C199, C200, C205, C204, C203, C202, C201
 with sigma of 0.01
 C208, C209, C214, C213, C212, C211, C210
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(O9) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(O16A) \\sim Ueq, Uanis(O16B)
\\sim Ueq: with sigma of 0.0025 and sigma for terminal atoms of 0.005
Uanis(C89) \\sim Ueq, Uanis(C88) \\sim Ueq, Uanis(C87) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O13A) = Uanis(O13B)
Uanis(O14A) = Uanis(O14B)
Uanis(O15A) = Uanis(O15B)
Uanis(O16A) = Uanis(O16B)
Uanis(C99) = Uanis(C199)
Uanis(C108) = Uanis(C208)
Uanis(C100) = Uanis(C200)
Uanis(C101) = Uanis(C205)
Uanis(C102) = Uanis(C204)
Uanis(C103) = Uanis(C203)
Uanis(C104) = Uanis(C202)
Uanis(C105) = Uanis(C201)
Uanis(C106) = Uanis(C206)
Uanis(C107) = Uanis(C207)
Uanis(C109) = Uanis(C209)
Uanis(C110) = Uanis(C214)
Uanis(C111) = Uanis(C213)
Uanis(C112) = Uanis(C212)
Uanis(C113) = Uanis(C211)
Uanis(C114) = Uanis(C210)
5. Rigid body (RIGU) restrains
 O10, O9, C83, C84, C89, C88, C87, C86, C85
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O13A, O14A, O15A, O16A, C99, C100, C101, C102, C103, C104, C105, C106, C107,
 C108, C109, C110, C111, C112, C113, C114, O13B, O14B, O15B, O16B, C199, C200,
 C201, C202, C203, C204, C205, C206, C207, C208, C209, C210, C211, C212, C213,
 C214
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Same fragment restrains
{O1, O2, O3, O4, C51, C52, C53, C54, C55, C56, C57, C58, C59, C60, C61, C62,
C63, C64, C65, C66} sigma for 1-2: 0.0125, 1-3: 0.04
as
{O13A, O14A, O15A, O16A, C99, C100, C101, C102, C103, C104, C105, C106, C107,
C108, C109, C110, C111, C112, C113, C114}
{O1, O2, O3, O4, C51, C52, C53, C54, C55, C56, C57, C58, C59, C60, C61, C62,
C63, C64, C65, C66} sigma for 1-2: 0.0125, 1-3: 0.04
as
{O13B, O14B, O15B, O16B, C199, C200, C201, C202, C203, C204, C205, C206, C207,
C208, C209, C210, C211, C212, C213, C214}
7. Others
 Fixed Sof: O13A(0.5) O14A(0.5) O15A(0.5) O16A(0.5) C99(0.5) C100(0.5)
 C101(0.5) H101(0.5) C102(0.5) H102(0.5) C103(0.5) C104(0.5) H104(0.5)
 C105(0.5) H105(0.5) C106(0.5) H106(0.5) C107(0.5) H107(0.5) C108(0.5)
 C109(0.5) C110(0.5) H110(0.5) C111(0.5) H111(0.5) C112(0.5) C113(0.5)
 H113(0.5) C114(0.5) H114(0.5) O13B(0.5) O14B(0.5) O15B(0.5) O16B(0.5)
 C199(0.5) C200(0.5) C201(0.5) H201(0.5) C202(0.5) H202(0.5) C203(0.5)
 C204(0.5) H204(0.5) C205(0.5) H205(0.5) C206(0.5) H206(0.5) C207(0.5)
 H207(0.5) C208(0.5) C209(0.5) C210(0.5) H210(0.5) C211(0.5) H211(0.5)
 C212(0.5) C213(0.5) H213(0.5) C214(0.5) H214(0.5)
8.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C37(H37A,H37B), C38(H38A,
 H38B), C39(H39A,H39B)
8.b 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), C26(H26), C27(H27), C29(H29), C30(H30), C32(H32), C41(H41),
  C42(H42), C44(H44), C45(H45), C47(H47), C53(H53), C54(H54), C56(H56),
 C57(H57), C58(H58), C59(H59), C62(H62), C63(H63), C65(H65), C66(H66), C69(H69),
  C70(H70), C72(H72), C73(H73), C74(H74), C75(H75), C78(H78), C79(H79),
 C81(H81), C82(H82), C85(H85), C86(H86), C88(H88), C89(H89), C90(H90), C91(H91),
  C94(H94), C95(H95), C97(H97), C98(H98), C101(H101), C102(H102), C104(H104),
 C105(H105), C106(H106), C107(H107), C110(H110), C111(H111), C113(H113),
 C114(H114), C201(H201), C202(H202), C204(H204), C205(H205), C206(H206),
 C207(H207), C210(H210), C211(H211), C213(H213), C214(H214)
8.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C25(H25A,H25B,H25C), C35(H35A,H35B,H35C), C50(H50A,H50B,
 H50C)
;
_shelx_res_checksum              48181
_shelx_hkl_checksum              55761
_shelx_fab_checksum              90106
_olex2_submission_special_instructions 'No special instructions were received'