[2 + 2] cycloaddition and its photomechanical effects on 1D coordination polymers with reversible amide bonds and coordination site regulation.
Wang, Lei; Qiao, Si-Bo; Chen, Yan-Ting; Ma, Xun; Wei, Wei-Ming; Zhang, Jun; Du, Lin; Zhao, Qi-Hua; Chemical science 15 (2024) 3971–3979; doi:10.1039/d3sc06098e

data_1570931
_publ_section_title
;
 [2 + 2] cycloaddition and its photomechanical effects on 1D coordination
 polymers with reversible amide bonds and coordination site regulation.
;
_journal_issue                   11
_journal_name_full               'Chemical science'
_journal_page_first              3971
_journal_page_last               3979
_journal_paper_doi               10.1039/d3sc06098e
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety
'C66 H52 Cd2 N8 O14 S4, 0.75(C2 H3 N), 0.25(H2 O)'
_chemical_formula_sum            'C67.5 H57.75 Cd2 N8.75 O14.25 S4'
_chemical_formula_weight         1572.51
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-06-30
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-09-20 deposited with the CCDC.	2024-02-05 downloaded from the CCDC.
;
_cell_angle_alpha                87.861(2)
_cell_angle_beta                 89.1320(10)
_cell_angle_gamma                85.016(2)
_cell_formula_units_Z            2
_cell_length_a                   12.5971(5)
_cell_length_b                   16.0044(8)
_cell_length_c                   16.5980(8)
_cell_measurement_reflns_used    9821
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      2.73
_cell_volume                     3331.1(3)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0741
_diffrn_reflns_av_unetI/netI     0.0420
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            125248
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.362
_diffrn_reflns_theta_min         1.977
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.837
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.7085
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0804 before and 0.0638 after correction.
The Ratio of minimum to maximum transmission is 0.9501.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_description       block
_exptl_crystal_F_000             1596
_refine_diff_density_max         1.361
_refine_diff_density_min         -1.132
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     923
_refine_ls_number_reflns         16644
_refine_ls_number_restraints     461
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0712
_refine_ls_R_factor_gt           0.0459
_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^)+(0.0491P)^2^+6.9337P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1055
_refine_ls_wR_factor_ref         0.1195
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12573
_reflns_number_total             16644
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc06098e6.cif
_cod_data_source_block           mo_230519c_0m
_cod_depositor_comments
'Adding full bibliography for 1570931--1570933.cif.'
_cod_original_formula_sum        'C67.50 H57.75 Cd2 N8.75 O14.25 S4'
_cod_database_code               1570931
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C69-C67
 1.48 with sigma of 0.01
 N68-C69
 1.15 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
S2 \\sim S3 \\sim C60 \\sim H60 \\sim C3 \\sim H3A \\sim H3B \\sim C49 \\sim
H49 \\sim C13 \\sim C53 \\sim C15 \\sim H15 \\sim H15A \\sim C63 \\sim H63
\\sim C65 \\sim H65 \\sim S3A \\sim C65A \\sim H65A \\sim C63A \\sim H63A \\sim
S2A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C69 \\sim N68 \\sim C67 \\sim O67A: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
Uanis(C69) \\sim Ueq, Uanis(N68) \\sim Ueq, Uanis(C67) \\sim Ueq, Uanis(O67A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(S2) \\sim Ueq, Uanis(S3) \\sim Ueq, Uanis(C60) \\sim Ueq, Uanis(C3) \\sim
Ueq, Uanis(C49) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C53) \\sim Ueq,
Uanis(C15) \\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(S3A)
\\sim Ueq, Uanis(C65A) \\sim Ueq, Uanis(C63A) \\sim Ueq, Uanis(S2A) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N68) \\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(C67) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 S2, S3, C60, H60, C3, H3A, H3B, C49, H49, C13, C53, C15, H15, H15A, C63, H63,
 C65, H65, S3A, C65A, H65A, C63A, H63A, S2A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C69, N68, C67, O67A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N68, C69, C67
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Others
 Sof(H15A)=Sof(S3A)=Sof(C65A)=Sof(H65A)=1-FVAR(1)
 Sof(S3)=Sof(H15)=Sof(C65)=Sof(H65)=FVAR(1)
 Sof(H3B)=Sof(C63A)=Sof(H63A)=Sof(S2A)=1-FVAR(2)
 Sof(S2)=Sof(H3A)=Sof(C63)=Sof(H63)=FVAR(2)
 Fixed Sof: C69(0.75) N68(0.75) C67(0.75) H67A(0.75) H67B(0.75) H67C(0.75)
 O67A(0.25) H67D(0.25) H67E(0.25)
6.a Riding coordinates:
 C67(H67A,H67B,H67C), O67A(H67D,H67E)
6.b Aromatic/amide H refined with riding coordinates:
 N2(H2), C1(H1), C4(H4), N5(H5), N3(H3), N7(H7), C16(H16), C24(H24), C26(H26),
 C28(H28), C34(H34), C36(H36), C38(H38), C44(H44), C50(H50), C54(H54), C56(H56),
  C58(H58), C60(H60), C62(H62), C66(H66), C33(H33), C17(H17), C9(H9), C37(H37),
 C5(H5A), C41(H41), C21(H21), C11(H11), C45(H45), C23(H23), C47(H47), C3(H3A),
 C3(H3B), C49(H49), C51(H51), C27(H27), C55(H55), C7(H7A), C29(H29), C59(H59),
 C15(H15), C15(H15A), C61(H61), C31(H31), C63(H63), C2(H2A), C65(H65),
 C65A(H65A), C63A(H63A)
6.c Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C57(H57A,H57B,H57C)
;
_shelx_res_checksum              77512
_olex2_submission_special_instructions 'No special instructions were received'