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_7244728
_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 N4 O14 Zn3, 2(C H4 O)'
_chemical_formula_sum            'C44 H40 N4 O16 Zn3'
_chemical_formula_weight         1076.91
_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   geom
_atom_sites_solution_primary     dual
_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                   11.17930(10)
_cell_length_b                   15.0014(2)
_cell_length_c                   25.5008(2)
_cell_measurement_reflns_used    21982
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      60.5440
_cell_measurement_theta_min      4.2240
_cell_volume                     4276.62(8)
_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_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_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 0.981
_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      1.00  95.00   0.50    0.10    --   73.55 -71.00 105.00  188
  2  \w    -71.00 -44.00   0.50    0.10    --  -74.80  38.00 -60.00   54
  3  \w    -71.00  -1.00   0.50    0.10    --  -74.80  38.00 -60.00  140
  4  \w    -26.00  -1.00   0.50    0.10    --  -74.80  38.00 -60.00   50
  5  \w    -73.00  16.00   0.50    0.05    --   -0.62 -57.00 150.00  178
  6  \w   -148.00 -56.00   0.50    0.10    --  -74.80 -65.00 -27.00  184
  7  \w   -148.00 -88.00   0.50    0.10    --  -74.80 -99.00  30.00  120
  8  \w   -148.00-103.00   0.50    0.10    --  -74.80 -99.00  90.00   90
  9  \w   -127.00-101.00   0.50    0.10    --  -74.80 -99.00-150.00   52
 10  \w   -148.00 -81.00   0.50    0.10    --  -74.80 -86.00-135.00  134
;
_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      0.0236226000
_diffrn_orient_matrix_UB_12      0.0704043000
_diffrn_orient_matrix_UB_13      -0.0305636000
_diffrn_orient_matrix_UB_21      -0.1042810000
_diffrn_orient_matrix_UB_22      -0.0118566000
_diffrn_orient_matrix_UB_23      -0.0249091000
_diffrn_orient_matrix_UB_31      -0.0540671000
_diffrn_orient_matrix_UB_32      0.0536022000
_diffrn_orient_matrix_UB_33      0.0346685000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_unetI/netI     0.0357
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            27223
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         60.699
_diffrn_reflns_theta_min         2.971
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    1.743
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58517
_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    1.673
_exptl_crystal_description       block
_exptl_crystal_F_000             2200
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.265
_refine_diff_density_min         -0.883
_refine_diff_density_rms         0.078
_refine_ls_abs_structure_details
;
 Flack x determined using 3530 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.013(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     612
_refine_ls_number_reflns         9299
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0361
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0412P)^2^+5.2685P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0889
_refine_ls_wR_factor_ref         0.0906
_reflns_Friedel_coverage         0.731
_reflns_Friedel_fraction_full    0.949
_reflns_Friedel_fraction_max     0.893
_reflns_number_gt                8781
_reflns_number_total             9299
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00088a2.cif
_cod_data_source_block           l-oh-bim+bdc+zn_autored
_cod_database_code               7244728
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'Zn C H O N'
_diffrn_oxdiff_digest_frames
;
01f4775b98ce361a80493b801f82fa396a0119079ea
;
_diffrn_oxdiff_digest_hkl
;
016b05f237f121857d4988adf1ad2e667e4bc5
;
_reflns_odcompleteness_completeness 99.86
_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
 O01O-C2
 1.37 with sigma of 0.002
3. Rigid bond restraints
 O01O, C2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O01O \\sim C2: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(O01O) \\sim Ueq, Uanis(C2) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
5.a Ternary CH refined with riding coordinates:
 C01D(H01D), C01I(H01I)
5.b Aromatic/amide H refined with riding coordinates:
 N00K(H00K), N00L(H00L), C00T(H00T), C00U(H00U), C010(H010), C011(H011),
 C013(H013), C016(H016), C017(H017), C019(H019), C01A(H01A), C01C(H01C),
 C01E(H01E), C01G(H01G), C01K(H01K), C01L(H01L), C01M(H01M), C01N(H01N),
 C01Q(H01Q), C01R(H01R), C01S(H01S), C01T(H01T)
5.c Idealised Me refined as rotating group:
 C01J(H01B,H01F,H01H), C01P(H01J,H01O,H01P), C01U(H01U,H01V,H01W), C2(H2A,H2B,
 H2C)
5.d Idealised tetrahedral OH refined as rotating group:
 O00H(H00H), O00I(H00I), O00M(H00M), O01O(H01X)
;
_shelx_res_checksum              95296
_shelx_hkl_checksum              29944
_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 1.566
_oxdiff_exptl_absorpt_empirical_full_min 0.545