Adaptive coordination assemblies based on a flexible tetraazacyclododecane ligand for promoting carbon dioxide fixation
Li, Shao-Chuan; Liu, Caiping; chen, qihui; Jiang, Feilong; Yuan, Daqiang; Sun, Qing-Fu; Hong, Maochun; Chemical Science  (2022) –; doi:10.1039/D2SC03093D

data_1567238
_publ_section_title
;
 Adaptive coordination assemblies based on a flexible
 tetraazacyclododecane ligand for promoting carbon dioxide fixation
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D2SC03093D
_journal_year                    2022
_chemical_formula_moiety         'C88 H144 Ag2 N24 Pd4, 4(O)'
_chemical_formula_sum            'C88 H144 Ag2 N24 O4 Pd4'
_chemical_formula_weight         2243.60
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-05-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-05-25 deposited with the CCDC.	2022-07-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.536(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   22.785(3)
_cell_length_b                   15.8669(17)
_cell_length_c                   20.292(2)
_cell_measurement_reflns_used    9904
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      2.40
_cell_volume                     6955.5(14)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      149.99
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            40648
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         3.107
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.824
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5759
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1182 before and 0.0714 after correction.
The Ratio of minimum to maximum transmission is 0.7724.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.071
_exptl_crystal_description       plate
_exptl_crystal_F_000             2300
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.716
_refine_diff_density_min         -1.961
_refine_diff_density_rms         0.217
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         7261
_refine_ls_number_restraints     295
_refine_ls_restrained_S_all      1.580
_refine_ls_R_factor_all          0.1255
_refine_ls_R_factor_gt           0.1138
_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^)+(0.1390P)^2^+235.0692P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2942
_refine_ls_wR_factor_ref         0.3068
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6243
_reflns_number_total             7261
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc03093d2.cif
_cod_data_source_block           2-SO42-
_cod_original_cell_volume        6955.4(13)
_cod_database_code               1567238
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.992
_shelx_estimated_absorpt_t_min   0.960
_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. Restrained distances
 N21-C24 = N21-C22 = N21-C23 = N8-C7 = N13-C14 = N25-C28 = N25-C27 = N25-C26
 1.47 with sigma of 0.005
 C24-N21
 2.45 with sigma of 0.01
 N25-C27 = N25-C26 = N25-C28 = N13-C14 = N8-C7 = N21-C24 = N21-C23 = N21-C22
 1.47 with sigma of 0.005
 C24-C24_$2 = C28_$1-C28_$3 = C24_$1-C24_$3 = C28-C28_$2
 1.53 with sigma of 0.005
 N25_$2-C27_$2 = N25_$2-C28_$2 = N25_$2-C26_$2 = N25-C26 = N25-C27 = N25-C28 =
 N21_$2-C24_$2 = N21-C24 = N21-C22 = N21-C23 = N21_$2-C23_$2 = N21_$2-C22_$2 =
 N21_$1-C23_$1 = N21_$1-C22_$1 = N21_$1-C24_$1 = N21_$3-C24_$3 = N21_$3-C22_$3 =
  N21_$3-C23_$3 = N25_$1-C28_$1 = N25_$1-C26_$1 = N25_$1-C27_$1 = N25_$3-C28_$3
 = N25_$3-C27_$3 = N25_$3-C26_$3 = N8_$1-C7_$1 = N13-C14 = N8-C7 = N13_$1-
 C14_$1 = N8_$3-C7_$3 = N13_$2-C14_$2 = N8_$2-C7_$2 = N13_$3-C14_$3
 1.46 with sigma of 0.005
 N21-C24 = N21-C23 = N21-C22 = N8-C7 = N8-C8 = N13-C14 = N13-C0AA = N25-C28 =
 N25-C27 = N25-C26
 1.465 with sigma of 0.005
 N21-C23 = N21-C22 = N21-C24 = N21_$2-C24_$2 = N21_$2-C23_$2 = N21_$2-C22_$2 =
 N21_$3-C23_$3 = N21_$3-C24_$3 = N21_$3-C22_$3 = N21_$1-C22_$1 = N21_$1-C24_$1 =
  N21_$1-C23_$1
 1.465 with sigma of 0.005
 C24_$3-C24_$1 = C24_$2-C24
 1.53 with sigma of 0.005
 N13-C0AA
 1.465 with sigma of 0.005
 N8-C7 = N8-C8 = N13-C0AA = N13-C14
 1.465 with sigma of 0.005
 N25-C26 = N25-C27 = N25-C28 = N21-C24 = N21-C23 = N21-C22
 1.465 with sigma of 0.005
 C8-C0AA
 1.53 with sigma of 0.005
 N8_$2-C10_$2 = N13_$3-C2AA_$2 = N8_$3-C10_$3 = N13_$2-C2AA_$3 = N13_$1-C2AA =
 N8-C10 = N13-C2AA_$1 = N8_$1-C10_$1
 1.465 with sigma of 0.005
 C2AA_$1-C10_$1 = C2AA-C10 = C2AA_$3-C10_$3 = C2AA_$2-C10_$2
 1.53 with sigma of 0.005
 C10_$1-C8_$1
 2.35 with sigma of 0.01
 C8-C10
 2.35 with sigma of 0.01
 C0AA-C2AA_$1
 2.35 with sigma of 0.01
 C0AA_$1-C2AA
 2.35 with sigma of 0.01
 C10_$3-C8_$3
 2.35 with sigma of 0.01
 C8_$2-C10_$2
 2.35 with sigma of 0.01
 C2AA_$2-C0AA_$3
 2.35 with sigma of 0.01
 C0AA_$2-C2AA_$3
 2.35 with sigma of 0.01
 C22-C23
 2.4 with sigma of 0.005
 C27-C28
 2.4 with sigma of 0.005
3. Rigid bond restraints
 C27, C28, C26, C22, C24, C23
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 N21
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
C22 \\sim C23 \\sim C27 \\sim C28 \\sim C26: within 2A with sigma of 0.005 and
sigma for terminal atoms of 0.01
Uanis(C28) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C22)
\\sim Ueq, Uanis(C23) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.01
Uanis(C23) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(N13)
\\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(N25) \\sim Ueq,
Uanis(C27) \\sim Ueq, Uanis(C6) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C8) \\sim Ueq, Uanis(C0AA) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C22) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(N21) \\sim Ueq, Uanis(C23)
\\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq:
with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C8) \\sim Ueq, Uanis(C0AA) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C27)
\\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C23) \\sim Ueq,
Uanis(C22) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C10) \\sim Ueq, Uanis(C2AA) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C2AA)
\\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C2AA) \\sim Ueq, Uanis(C2AA) \\sim Ueq,
Uanis(C10) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C0AA) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C2AA) \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.01
Uanis(C2AA) \\sim Ueq, Uanis(C0AA) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C10) \\sim Ueq, Uanis(C2AA) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C0AA)
\\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C27) \\sim Ueq,
Uanis(C23) \\sim Ueq, Uanis(C22) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C2) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O1) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C23)
\\sim Ueq, Uanis(C2AA) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq,
Uanis(C28) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C0AA)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
5.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C14(H14A,H14B), C24(H24A,H24B), C28(H28A,H28B), C0AA(H0AA,H0AB),
 C8(H8A,H8B), C2AA(H2AA,H2AB), C10(H10A,H10B)
5.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C16(H16), C19(H19), C6(H6), C20(H20), C3(H3), C5(H5), C2(H2)
5.c Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C23(H23B,H23A,H23C), C26(H26A,H26B,H26C), C22(H22A,H22B,
 H22C)
;
_shelx_res_checksum              12873
_shelx_fab_checksum              59972
_olex2_submission_special_instructions 'No special instructions were received'