Photomechanical behavior triggered by [2 + 2] cycloaddition and photochromism of pyridinium-functionalized coordination complex
Chen, Yun-Rui; Jia, Meng-Ze; Pan, Jia-Qi; Tan, Bin; Zhang, Jie; Dalton Transactions  (2022) –; doi:10.1039/D2DT00599A

data_7709839
_publ_section_title
;
 Photomechanical behavior triggered by [2 + 2] cycloaddition and
 photochromism of pyridinium-functionalized coordination complex
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00599A
_journal_year                    2022
_chemical_formula_moiety         'C40 H40 N4 O8 Zn, O4 S, 9[H2O]'
_chemical_formula_sum            'C40 H40 N4 O12 S Zn'
_chemical_formula_weight         866.19
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2022-03-16
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-03-17 deposited with the CCDC.	2022-03-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.576(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.7108(17)
_cell_length_b                   27.961(2)
_cell_length_c                   13.5892(13)
_cell_measurement_reflns_used    6274
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.7060
_cell_measurement_theta_min      3.9630
_cell_volume                     4999.0(10)
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_unetI/netI     0.0335
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            24513
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.500
_diffrn_reflns_theta_min         3.423
_exptl_absorpt_coefficient_mu    0.588
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.151
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1800
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.542
_refine_diff_density_min         -0.230
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     461
_refine_ls_number_reflns         5144
_refine_ls_number_restraints     240
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0439
_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^)+(0.0762P)^2^+2.2182P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1240
_refine_ls_wR_factor_ref         0.1374
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3921
_reflns_number_total             5144
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00599a2.cif
_cod_data_source_block           Zn-bpe
_cod_original_cell_volume        4999.1(10)
_cod_database_code               7709839
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Restrained distances
 O1W-H1WA = O1W-H1WB
 0.85 with sigma of 0.02
 O2W-H2WA = O2W-H2WB
 0.85 with sigma of 0.02
 H2WA-H2WB
 1.34 with sigma of 0.04
 H1WA-H1WB
 1.34 with sigma of 0.04
 S1-O3 \\sim S1-O4 \\sim S1-O5 \\sim S1-O6
 with sigma of 0.02
 N2-C10 \\sim N2A-C11A
 with sigma of 0.02
 O3-O5 \\sim O4-O6 \\sim O3-O6 \\sim O4-O5 \\sim O3-O4 \\sim O5-O6
 with sigma of 0.04
 N2-C11 \\sim N2A-C10A
 with sigma of 0.02
 C4-C6 \\sim C2A-C6A
 with sigma of 0.04
 C7-C9 \\sim C7A-C12A
 with sigma of 0.04
 C9-C12 \\sim C12A-C9A
 with sigma of 0.04
 C1-C2 \\sim C5A-C4A
 with sigma of 0.02
 C2-C3 \\sim C4A-C3A
 with sigma of 0.02
 C3-C4 \\sim C3A-C2A
 with sigma of 0.02
 C3-C6 \\sim C3A-C6A
 with sigma of 0.02
 Zn1-N1 \\sim Zn1-N1A
 with sigma of 0.02
 C6-C7 \\sim C6A-C7A
 with sigma of 0.02
 C7-C8 \\sim C7A-C8A
 with sigma of 0.02
 C10-C11 \\sim C11A-C10A
 with sigma of 0.04
 C8-C9 \\sim C8A-C12A
 with sigma of 0.02
 C8-C12 \\sim C8A-C9A
 with sigma of 0.02
 N1-C1 \\sim N1A-C5A
 with sigma of 0.02
 N1-C5 \\sim N1A-C1A
 with sigma of 0.02
 C3-C7 \\sim C3A-C7A
 with sigma of 0.04
 C8-C10 \\sim C8A-C11A
 with sigma of 0.04
 C4-C5 \\sim C2A-C1A
 with sigma of 0.02
 C11-C12 \\sim C10A-C9A
 with sigma of 0.02
 C6-C8 \\sim C6A-C8A
 with sigma of 0.04
 Zn1-C1 \\sim Zn1-C5A
 with sigma of 0.04
 Zn1-C5 \\sim Zn1-C1A
 with sigma of 0.04
 C7-C12 \\sim C7A-C9A
 with sigma of 0.04
 N1-C2 \\sim N1A-C4A
 with sigma of 0.04
 N1-C4 \\sim N1A-C2A
 with sigma of 0.04
 C8-C11 \\sim C8A-C10A
 with sigma of 0.04
 N2-C9 \\sim N2A-C12A
 with sigma of 0.04
 N2-C12 \\sim N2A-C9A
 with sigma of 0.04
 C1-C3 \\sim C5A-C3A
 with sigma of 0.04
 C1-C5 \\sim C5A-C1A
 with sigma of 0.04
 C2-C4 \\sim C4A-C2A
 with sigma of 0.04
 C2-C6 \\sim C4A-C6A
 with sigma of 0.04
 C9-C10 \\sim C12A-C11A
 with sigma of 0.02
 C3-C5 \\sim C3A-C1A
 with sigma of 0.04
 O4-O5 \\sim O4A-O5A
 with sigma of 0.04
 O4-O6 \\sim O4A-O6A
 with sigma of 0.04
 O5-O6 \\sim O5A-O6A
 with sigma of 0.04
 O3-O4 \\sim O3A-O4A
 with sigma of 0.04
 O3-O5 \\sim O3A-O5A
 with sigma of 0.04
 O3-O6 \\sim O3A-O6A
 with sigma of 0.04
 Zn1-H1WA \\sim Zn1-H1WB
 with sigma of 0.02
 Zn1-H2WA \\sim Zn1-H2WB
 with sigma of 0.02
2. Rigid bond restraints
 C2, C3
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.01
 C8, C12
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
S1 \\sim O3 \\sim O4 \\sim O5 \\sim O6: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
C8 \\sim C12: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.01
within 2A
Uanis(S1) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O5) \\sim
Ueq, Uanis(O6) \\sim Ueq, Uanis(O5A) \\sim Ueq, Uanis(O4A) \\sim Ueq,
Uanis(O3A) \\sim Ueq, Uanis(O6A) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C4A) \\sim Ueq, Uanis(C5A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 S1, O3, O4, O5, O6
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O3A, O4A, O5A, O6A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(N1A)=Sof(N2A)=Sof(C1A)=Sof(H1A)=Sof(C2A)=Sof(H2A)=Sof(C3A)=Sof(C4A)=
 Sof(H4A)=Sof(C5A)=Sof(H5A)=Sof(C6A)=Sof(H6A)=Sof(C7A)=Sof(H7A)=Sof(C8A)=
 Sof(C9A)=Sof(H9A)=Sof(C10A)=Sof(H10A)=Sof(C11A)=Sof(H11A)=Sof(C12A)=Sof(H12A)=
 Sof(H13D)=Sof(H13C)=1-FVAR(1)
 Sof(N1)=Sof(N2)=Sof(C1)=Sof(H1)=Sof(C2)=Sof(H2)=Sof(C3)=Sof(C4)=Sof(H4)=
 Sof(C5)=Sof(H5)=Sof(C6)=Sof(H6)=Sof(C7)=Sof(H7)=Sof(C8)=Sof(C9)=Sof(H9)=
 Sof(C10)=Sof(H10)=Sof(C11)=Sof(H11)=Sof(C12)=Sof(H12)=Sof(H13A)=Sof(H13B)=
 FVAR(1)
 Fixed Sof: S1(0.5) O3(0.25) O3A(0.25) O4(0.25) O4A(0.25) O5(0.25) O5A(0.25)
 O6(0.25) O6A(0.25)
6.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C13(H13D,H13C)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C1A(H1A), C2(H2), C2A(H2A), C4(H4), C4A(H4A), C5(H5), C5A(H5A),
 C6(H6), C6A(H6A), C7(H7), C7A(H7A), C9(H9), C9A(H9A), C10(H10), C10A(H10A),
 C11(H11), C11A(H11A), C12(H12), C12A(H12A), C15(H15), C16(H16), C18(H18),
 C19(H19)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 364 electrons were 
found in a volume of 1298\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
9[H2O] per Asymmetric Unit 
which account for 360 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              79896
_shelx_fab_checksum              99804
_olex2_submission_special_instructions 'No special instructions were received'