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_1567239
_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 H148 Ag2 N24 O2 Pd4, 2(F6 Si), 2(B F4)'
_chemical_formula_sum            'C88 H148 Ag2 B2 F20 N24 O2 Pd4 Si2'
_chemical_formula_weight         2673.44
_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     iterative
_audit_creation_date             2022-03-20
_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                72.754(2)
_cell_angle_beta                 73.765(2)
_cell_angle_gamma                80.009(2)
_cell_formula_units_Z            1
_cell_length_a                   13.5019(3)
_cell_length_b                   14.0260(3)
_cell_length_c                   20.0093(5)
_cell_measurement_reflns_used    33626
_cell_measurement_temperature    105.1(2)
_cell_measurement_theta_max      60.6430
_cell_measurement_theta_min      2.0720
_cell_volume                     3457.63(15)
_computing_cell_refinement       'CrysAlisPro 1.171.40.59a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.59a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.59a (Rigaku OD, 2019)'
_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_environment      N~2~
_diffrn_ambient_temperature      105.1(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -16.00  70.00   0.50    0.05    --   -1.72  57.00 -60.00  172
  2  \w     33.00  58.00   0.50    0.05    --   -1.72  38.00 -30.00   50
  3  \w     33.00  61.00   0.50    0.05    --   -1.72  77.00  90.00   56
  4  \w     75.00 111.00   0.50    0.05    --   72.03 152.00 -16.00   72
  5  \w     82.00 122.00   0.50    0.05    --   72.03 121.00-176.00   80
  6  \w     57.00 143.00   0.50    0.05    --   72.03  57.00-180.00  172
  7  \w     58.00 101.00   0.50    0.05    --   72.03-125.00 -60.00   86
  8  \w     58.00  83.00   0.50    0.05    --   72.03-152.00 -59.00   50
  9  \w      5.00  63.00   0.50    0.05    --   72.03 -57.00 -60.00  116
 10  \w      0.00  95.00   0.50    0.05    --   72.03 -77.00 -60.00  190
 11  \w     19.00 100.00   0.50    0.05    --   72.03-121.00 100.00  162
 12  \w     41.00  66.00   0.50    0.05    --   72.03 -57.00 120.00   50
 13  \w     13.00  66.00   0.50    0.05    --   72.03 -57.00  90.00  106
 14  \w      1.00  27.00   0.50    0.05    --   72.03 -57.00 120.00   52
 15  \w     -1.00  85.00   0.50    0.05    --   72.03 -77.00  90.00  172
 16  \w      0.00  26.00   0.50    0.05    --   72.03 -19.00   0.00   52
 17  \w     -1.00  26.00   0.50    0.05    --   72.03 -19.00 -60.00   54
 18  \w     -1.00  61.00   0.50    0.05    --   72.03 -57.00-120.00  124
 19  \w      0.00  25.00   0.50    0.05    --   72.03 -19.00-120.00   50
 20  \w    -16.00  10.00   0.50    0.05    --   -1.72  77.00  90.00   52
 21  \w    -72.00   8.00   0.50    0.05    --   -1.72 -38.00 150.00  160
 22  \w    -43.00 -10.00   0.50    0.05    --  -75.46  38.00  30.00   66
 23  \w    -43.00  -6.00   0.50    0.05    --  -75.46  38.00 -60.00   74
 24  \w    -37.00 -12.00   0.50    0.05    --  -75.46  38.00-150.00   50
 25  \w    -26.00   0.00   0.50    0.05    --  -75.46  19.00-180.00   52
 26  \w    -63.00  -2.00   0.50    0.05    --  -75.46  57.00-150.00  122
 27  \w    -62.00 -21.00   0.50    0.05    --  -75.46  77.00   0.00   82
 28  \w    -26.00   0.00   0.50    0.05    --  -75.46  19.00 150.00   52
 29  \w   -115.00 -84.00   0.50    0.05    --  -75.46-121.00 100.00   62
 30  \w   -129.00 -53.00   0.50    0.05    --  -75.46 -77.00  30.00  152
 31  \w   -109.00 -84.00   0.50    0.05    --  -75.46-152.00 -59.00   50
 32  \w   -109.00 -33.00   0.50    0.05    --  -75.46 121.00-176.00  152
 33  \w   -130.00 -69.00   0.50    0.05    --  -75.46 152.00 -16.00  122
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0377489000
_diffrn_orient_matrix_UB_12      -0.0078401000
_diffrn_orient_matrix_UB_13      0.0567909000
_diffrn_orient_matrix_UB_21      0.0808683000
_diffrn_orient_matrix_UB_22      0.0484174000
_diffrn_orient_matrix_UB_23      -0.0439811000
_diffrn_orient_matrix_UB_31      -0.0530344000
_diffrn_orient_matrix_UB_32      0.0876797000
_diffrn_orient_matrix_UB_33      0.0076583000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.0804
_diffrn_reflns_av_unetI/netI     0.0522
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            46670
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        52.931
_diffrn_reflns_theta_max         52.931
_diffrn_reflns_theta_min         3.189
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    4.816
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56799
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.59a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_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    1.284
_exptl_crystal_description       block
_exptl_crystal_F_000             1356
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.25
_refine_diff_density_max         3.395
_refine_diff_density_min         -2.193
_refine_diff_density_rms         0.197
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     658
_refine_ls_number_reflns         12164
_refine_ls_number_restraints     196
_refine_ls_restrained_S_all      1.626
_refine_ls_R_factor_all          0.0840
_refine_ls_R_factor_gt           0.0800
_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^)+(0.1198P)^2^+32.2581P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2111
_refine_ls_wR_factor_ref         0.2144
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11075
_reflns_number_total             12164
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc03093d2.cif
_cod_data_source_block           2-BF4
_cod_database_code               1567239
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_usercomment     'C H O N Pd'
_shelx_estimated_absorpt_t_max   0.379
_shelx_estimated_absorpt_t_min   0.197
_diffrn_oxdiff_digest_frames
;
014a15a68038f3467a877aba0c691e0ac003114f387
;
_diffrn_oxdiff_digest_hkl
;
01f7274b60d799f71e25286ae97fe4d9bf6365
;
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     56.82
_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, All O(H,H) groups
2. Restrained distances
 C2BA-C1BA = C4-C3BA = C7-C3 = C9AA-C0BA
 1.53 with sigma of 0.005
 N11-C2BA = N11-C4 = N8-C3BA = N8-C3 = N17-C7 = N17-C9AA = N14-C0BA = N14-C1BA
 1.47 with sigma of 0.005
 N7_$1-C4AA_$1 = N4_$1-C7AA_$1 = N4_$1-C9_$1 = N4_$1-C5AA_$1 = N7_$1-C11_$1 =
 N7_$1-C10_$1 = N12_$1-C13_$1 = N15_$1-C14_$1 = N15_$1-C19_$1 = N15_$1-C18_$1 =
 N12_$1-C16_$1 = N12_$1-C17_$1 = N12-C13 = N12-C16 = N12-C17 = N15-C14 = N15-
 C18 = N15-C19 = N4-C7AA = N7-C4AA = N7-C10 = N7-C11 = N4-C9 = N4-C5AA = N11-
 C2BA = N11-C20 = N11-C4 = N8-C8AA = N8-C3BA = N8-C3 = N14-C27 = N14-C0BA = N14-
 C1BA = N17-C9AA = N17-C34 = N17-C7 = N8_$1-C3_$1 = N8_$1-C8AA_$1 = N8_$1-
 C3BA_$1 = N17_$1-C34_$1 = N17_$1-C9AA_$1 = N17_$1-C7_$1 = N14_$1-C1BA_$1 =
 N14_$1-C27_$1 = N14_$1-C0BA_$1 = N11_$1-C20_$1 = N11_$1-C4_$1 = N11_$1-C2BA_$1
 1.47 with sigma of 0.005
 C7AA-C4AA = C14-C13 = C7AA_$1-C4AA_$1 = C14_$1-C13_$1 = C7_$1-C3_$1 = C9AA_$1-
 C0BA_$1 = C4_$1-C3BA_$1 = C2BA_$1-C1BA_$1 = C7-C3 = C4-C3BA = C2BA-C1BA = C9AA-
 C0BA
 1.53 with sigma of 0.005
 N14-C27 = N8-C8AA = N8-C3BA = N8-C3 = N14-C1BA = N14-C0BA = N11-C20 = N11-C4 =
  N11-C2BA = N17-C34 = N17-C9AA = N17-C7 = N15-C19 = N15-C18 = N15-C14 = N12-
 C13 = N12-C16 = N12-C17 = N7-C4AA = N4-C7AA = N7-C11 = N7-C10 = N4-C5AA = N4-C9
 1.475 with sigma of 0.005
 H3A-H1BA
 2.45 with sigma of 0.005
 H4A-H9AA
 2.45 with sigma of 0.005
 H3A-H4A
 2.45 with sigma of 0.01
 H3A-H9AA
 2.45 with sigma of 0.01
 H1BA-H9AA
 2.45 with sigma of 0.01
 H1BA-H4A
 2.45 with sigma of 0.01
3. Rigid bond restraints
 C3BA, C4, C2BA, C1BA, C3, C7, C9AA, C0BA
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C2BA, C1BA, C0BA, C9AA, C7, C3, C3BA, C4
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 N14, N14, C1BA, C1BA
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 N17, N17, C9AA, C9AA
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 N11, N11, C4, C4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 N8, N8, C3, C3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C2BA, C1BA, C3, C7, N8, N14
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 N11, C4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 N17, C9AA
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
C4 \\sim C3BA \\sim C7 \\sim C3 \\sim C2BA \\sim C1BA \\sim C0BA \\sim C9AA:
within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(N17) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C4) \\sim Ueq, Uanis(C3BA) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C7)
\\sim Ueq, Uanis(C9AA) \\sim Ueq, Uanis(C0BA) \\sim Ueq, Uanis(C1BA) \\sim Ueq,
Uanis(C2BA) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(N11) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5.a Rotating group:
 O1(H1A,H1B)
5.b Secondary CH2 refined with riding coordinates:
 C8AA(H8AA,H8AB), C27(H27A,H27B), C20(H20A,H20B), C34(H34A,H34B), C4AA(H4AA,
 H4AB), C13(H13A,H13B), C7AA(H7AA,H7AB), C14(H14A,H14B), C1BA(H1BA,H1BB),
 C3(H3A,H3B), C4(H4A,H4B), C7(H7A,H7B), C9AA(H9AA,H9AB), C3BA(H3BA,H3BB),
 C2BA(H2BA,H2BB), C0BA(H0BA,H0BB)
5.c Aromatic/amide H refined with riding coordinates:
 C0AA(H0AA), C32(H32), C33(H33), C1AA(H1AA), C30(H30), C26(H26), C29(H29),
 C23(H23), C22(H22), C6AA(H6AA), C2AA(H2AA), C38(H38), C35(H35), C25(H25),
 C36(H36), C39(H39)
5.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C10(H10A,H10B,H10C), C5AA(H5AA,H5AB,H5AC), C9(H9A,H9B,
 H9C), C18(H18A,H18B,H18C), C11(H11A,H11B,H11C), C17(H17A,H17B,H17C), C19(H19A,
 H19B,H19C)
;
_shelx_res_checksum              46845
_shelx_fab_checksum              16111
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.240
_oxdiff_exptl_absorpt_empirical_full_min 0.303