Design Syntheses of Metal-Organic Layer with Rich N-sites for CO2 Chemical Fixation
Wang, Zhi-Wen; Zhu, Zi-Yi; Li, Shangda; Wang, Fei; CrystEngComm  (2022) –; doi:10.1039/D2CE00088A

data_7244725
_publ_section_title
;
 Design Syntheses of Metal-Organic Layer with Rich N-sites for CO2
 Chemical Fixation
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00088A
_journal_year                    2022
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C42 H32 Cd3 N4 O14, 2(C H4 O)'
_chemical_formula_sum            'C44 H40 Cd3 N4 O16'
_chemical_formula_weight         1218.00
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-11-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-11-24 deposited with the CCDC.	2022-04-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.52890(10)
_cell_length_b                   15.10390(10)
_cell_length_c                   26.52250(10)
_cell_measurement_reflns_used    53462
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      60.5830
_cell_measurement_theta_min      2.5420
_cell_volume                     4618.40(5)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_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   -111.00 -24.00   0.50    0.05    --  -75.22 125.00 120.00  174
  2  \w    -73.00  23.00   0.50    0.05    --   -0.94 -76.00  -6.00  192
  3  \w     10.00  93.00   0.50    0.05    --   73.34 -76.00  -6.00  166
  4  \w     80.00 146.00   0.50    0.05    --   73.34 125.00  60.00  132
  5  \w     50.00 145.00   0.50    0.05    --   73.34  76.00 120.00  190
  6  \w   -143.00 -54.00   0.50    0.05    --  -75.22 -76.00  -6.00  178
  7  \w    -84.00 -59.00   0.50    0.05    --  -75.22 -57.00-150.00   50
  8  \w   -146.00-112.00   0.50    0.05    --  -75.22 -57.00-150.00   68
  9  \w   -140.00 -99.00   0.50    0.05    --  -75.22 -99.00-150.00   82
 10  \w   -147.00 -88.00   0.50    0.05    --  -75.22 -99.00 -90.00  118
 11  \w   -131.00 -79.00   0.50    0.05    --  -75.22-125.00  90.00  104
 12  \w    -90.00 -25.00   0.50    0.05    --  -75.22  57.00 -30.00  130
 13  \w    -67.00 -37.00   0.50    0.05    --  -75.22  57.00  30.00   60
 14  \w    -90.00  -2.00   0.50    0.05    --  -75.22  57.00  90.00  176
 15  \w    -33.00  -7.00   0.50    0.05    --  -75.22  76.00 120.00   52
 16  \w    -91.00  -2.00   0.50    0.05    --  -75.22  57.00 120.00  178
 17  \w    -89.00 -63.00   0.50    0.05    --  -75.22  76.00 120.00   52
 18  \w    -18.00  58.00   0.50    0.05    --   -0.94  76.00 120.00  152
 19  \w    -68.00 -20.00   0.50    0.05    --  -75.22  38.00 -60.00   96
 20  \w     27.00  70.00   0.50    0.05    --   -0.94  38.00 -90.00   86
 21  \w     65.00 106.00   0.50    0.05    --   73.34 -99.00 -60.00   82
 22  \w     22.00 105.00   0.50    0.05    --   73.34-125.00-120.00  166
 23  \w      3.00  29.00   0.50    0.05    --   73.34 -99.00 -60.00   52
 24  \w     22.00  72.00   0.50    0.05    --   73.34-125.00 -30.00  100
 25  \w     77.00 110.00   0.50    0.05    --   73.34-125.00 -30.00   66
;
_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      -0.0936080000
_diffrn_orient_matrix_UB_12      0.0340508000
_diffrn_orient_matrix_UB_13      0.0227304000
_diffrn_orient_matrix_UB_21      0.0681329000
_diffrn_orient_matrix_UB_22      0.0365699000
_diffrn_orient_matrix_UB_23      0.0352183000
_diffrn_orient_matrix_UB_31      0.0095787000
_diffrn_orient_matrix_UB_32      0.0732200000
_diffrn_orient_matrix_UB_33      -0.0281627000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.0376
_diffrn_reflns_av_unetI/netI     0.0218
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            70674
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         60.595
_diffrn_reflns_theta_min         2.897
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    7.895
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.37061
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.752
_exptl_crystal_description       block
_exptl_crystal_F_000             2416
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.356
_refine_diff_density_min         -0.724
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details
;
 Flack x determined using 4246 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.014(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     616
_refine_ls_number_reflns         10522
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0221
_refine_ls_R_factor_gt           0.0203
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0265P)^2^+0.5960P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0491
_refine_ls_wR_factor_ref         0.0498
_reflns_Friedel_coverage         0.798
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.984
_reflns_number_gt                9915
_reflns_number_total             10522
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00088a2.cif
_cod_data_source_block           w3-38-10-d_autored
_cod_database_code               7244725
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'Cd C O N'
_shelx_estimated_absorpt_t_max   0.307
_shelx_estimated_absorpt_t_min   0.205
_diffrn_oxdiff_digest_frames
;
018284dbcb9e21eb47dbd554a63c23941702902bf46
;
_diffrn_oxdiff_digest_hkl
;
014b9ce7edecc750ac02d06a17e3562a18210f
;
_reflns_odcompleteness_completeness 99.94
_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 N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O00E-H00E
 0.85 with sigma of 0.01
 O00G-H00G
 0.85 with sigma of 0.01
 C01V-O01M
 1.35 with sigma of 0.002
 C00W-H00E
 1.881369 with sigma of 0.02
 Cd02-H00E
 3.143682 with sigma of 0.02
 C01B-H00G
 1.909493 with sigma of 0.02
 Cd03-H00G
 3.212405 with sigma of 0.02
3. Rigid bond restraints
 C01V, O01M
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C01V \\sim O01M: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(C01V) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5.a Ternary CH refined with riding coordinates:
 C00W(H00W), C01B(H01B)
5.b Aromatic/amide H refined with riding coordinates:
 N00A(H00A), C00P(H00P), C00R(H00R), C00Y(H00Y), C011(H011), C012(H012),
 C014(H014), N016(H016), C018(H018), C019(H019), C01A(H01A), C01C(H01C),
 C01D(H01D), C01E(H01E), C01F(H01F), C01I(H01I), C01K(H01K), C01N(H01N),
 C01O(H01O), C01P(H01P), C01Q(H01Q), C01R(H01R)
5.c Idealised Me refined as rotating group:
 C01S(H01T,H01U,H01V), C01T(H01G,H01H,H01J), C01U(H01L,H01M,H01S), C01V(H01X,
 H01Y,H)
5.d Idealised tetrahedral OH refined as rotating group:
 O00Z(H00Z), O01M(H01W)
;
_shelx_res_checksum              12211
_shelx_hkl_checksum              27913
_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 1.950
_oxdiff_exptl_absorpt_empirical_full_min 0.665