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_7244726
_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            'C43 H40 Cd3 N4 O16'
_chemical_formula_weight         1205.99
_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
_atom_sites_solution_primary     iterative
_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                   11.52880(10)
_cell_length_b                   15.09090(10)
_cell_length_c                   26.5164(2)
_cell_measurement_reflns_used    18610
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      60.5140
_cell_measurement_theta_min      2.5190
_cell_volume                     4613.32(6)
_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    'olex2.solve (Bourhis et al., 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 0.999
_diffrn_measured_fraction_theta_max 0.975
_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     86.00 111.00   0.50    0.05    --   73.42-125.00 -90.00   50
  2  \w     14.00  40.00   0.50    0.05    --   -0.78  38.00-180.00   52
  3  \w     37.00  87.00   0.50    0.05    --   73.42 -19.00  26.00  100
  4  \w   -103.00 -40.00   0.50    0.05    --  -74.98 171.00  69.00  126
  5  \w   -137.00-111.00   0.50    0.05    --  -74.98 171.00  69.00   52
  6  \w    -88.00 -25.00   0.50    0.05    --  -74.98  57.00 -30.00  126
  7  \w    -67.00 -10.00   0.50    0.05    --  -74.98  38.00 -30.00  114
  8  \w    -66.00   5.00   0.50    0.05    --   -0.78 -38.00-120.00  142
  9  \w   -144.00 -86.00   0.50    0.05    --  -74.98-113.00 -70.00  116
;
_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      0.1033311000
_diffrn_orient_matrix_UB_12      0.0070949000
_diffrn_orient_matrix_UB_13      -0.0227245000
_diffrn_orient_matrix_UB_21      -0.0490643000
_diffrn_orient_matrix_UB_22      -0.0210482000
_diffrn_orient_matrix_UB_23      -0.0441605000
_diffrn_orient_matrix_UB_31      -0.0203841000
_diffrn_orient_matrix_UB_32      0.0859622000
_diffrn_orient_matrix_UB_33      -0.0089656000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_unetI/netI     0.0389
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            19974
_diffrn_reflns_point_group_measured_fraction_full 0.941
_diffrn_reflns_point_group_measured_fraction_max 0.888
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         60.566
_diffrn_reflns_theta_min         2.898
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    7.903
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38457
_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    1.736
_exptl_crystal_description       block
_exptl_crystal_F_000             2392
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.672
_refine_diff_density_min         -2.329
_refine_diff_density_rms         0.197
_refine_ls_abs_structure_details
;
 Flack x determined using 3391 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.008(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     616
_refine_ls_number_reflns         9425
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0444
_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^)+(0.0882P)^2^+1.1190P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1202
_refine_ls_wR_factor_ref         0.1213
_reflns_Friedel_coverage         0.647
_reflns_Friedel_fraction_full    0.868
_reflns_Friedel_fraction_max     0.781
_reflns_number_gt                9083
_reflns_number_total             9425
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00088a2.cif
_cod_data_source_block           l-oh-bim+bdc+cd-da_autored
_cod_database_code               7244726
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'Cd C H O N'
_diffrn_oxdiff_digest_frames
;
01fe337b3844d9dd3fabcd438d7c880680008784711
;
_diffrn_oxdiff_digest_hkl
;
01e9824275376a5ebe712856660820b8060afa
;
_reflns_odcompleteness_completeness 99.83
_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
 O00F-H00F
 0.85 with sigma of 0.01
 O00K-H00K
 0.85 with sigma of 0.01
 C01V-O01F
 1.37 with sigma of 0.002
 C014-H00F
 1.876694 with sigma of 0.02
 Cd03-H00F
 3.137199 with sigma of 0.02
 C019-H00K
 1.900735 with sigma of 0.02
 Cd02-H00K
 3.201457 with sigma of 0.02
3. Rigid bond restraints
 O01F, C01V
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O01F \\sim C01V: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
5.a Ternary CH refined with riding coordinates:
 C014(H014), C019(H019)
5.b Aromatic/amide H refined with riding coordinates:
 N00E(H00E), C00R(H00R), C00T(H00T), C00U(H00U), C00W(H00W), C00X(H00X),
 C011(H011), N017(H017), C018(H018), C01A(H01A), C01D(H01D), C01E(H01E),
 C01H(H01H), C01I(H01I), C01J(H01J), C01K(H01K), C01M(H01M), C01N(H01N),
 C01O(H01O), C01P(H01P), C01Q(H01Q), C01R(H01R)
5.c Idealised Me refined as rotating group:
 C01L(H01B,H01C,H01F), C01S(H01U,H01V,H01W), C01U(H01G,H01L,H01S), C01V(H01Y,H,
 HA)
5.d Idealised tetrahedral OH refined as rotating group:
 O01B(H01T), O01F(H01X)
;
_shelx_res_checksum              80153
_shelx_hkl_checksum              79117
_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 1.747
_oxdiff_exptl_absorpt_empirical_full_min 0.596