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_7244727
_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, C H4 O, C H O'
_chemical_formula_sum            'C44 H37 N4 O16 Zn3'
_chemical_formula_weight         1073.88
_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
_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                   11.18090(10)
_cell_length_b                   15.00360(10)
_cell_length_c                   25.50610(10)
_cell_measurement_reflns_used    27653
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      60.3810
_cell_measurement_theta_min      2.5440
_cell_volume                     4278.74(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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(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 0.986
_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    -15.00  73.00   0.50    0.05    --   -0.62  38.00  60.00  176
  2  \w    -94.00  -2.00   0.50    0.05    --  -74.78  66.00  86.00  184
  3  \w    -71.00  -1.00   0.50    0.05    --  -74.78  38.00  30.00  140
  4  \w    -17.00  72.00   0.50    0.05    --   -0.62  57.00 -90.00  178
  5  \w    -15.00  73.00   0.50    0.05    --   -0.62  38.00-180.00  176
  6  \w   -148.00 -88.00   0.50    0.05    --  -74.78 -99.00  90.00  120
  7  \w   -148.00 -81.00   0.50    0.05    --  -74.78 -85.00  76.00  134
  8  \w   -148.00 -88.00   0.50    0.05    --  -74.78 -99.00   0.00  120
  9  \w   -148.00 -88.00   0.50    0.05    --  -74.78 -99.00 -30.00  120
 10  \w   -148.00 -54.00   0.50    0.05    --  -74.78 -71.00-176.00  188
;
_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      -0.0861490000
_diffrn_orient_matrix_UB_12      -0.0564032000
_diffrn_orient_matrix_UB_13      -0.0151940000
_diffrn_orient_matrix_UB_21      -0.0295665000
_diffrn_orient_matrix_UB_22      0.0554241000
_diffrn_orient_matrix_UB_23      -0.0390354000
_diffrn_orient_matrix_UB_31      0.0778338000
_diffrn_orient_matrix_UB_32      -0.0413178000
_diffrn_orient_matrix_UB_33      -0.0316703000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.0198
_diffrn_reflns_av_unetI/netI     0.0202
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            30314
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         60.486
_diffrn_reflns_theta_min         2.971
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    1.742
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.18346
_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    1.667
_exptl_crystal_description       block
_exptl_crystal_F_000             2188
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.332
_refine_diff_density_min         -0.725
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details
;
 Flack x determined using 3683 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.004(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     611
_refine_ls_number_reflns         9259
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.155
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0311
_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^)+(0.0258P)^2^+6.9004P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0757
_refine_ls_wR_factor_ref         0.0761
_reflns_Friedel_coverage         0.725
_reflns_Friedel_fraction_full    0.964
_reflns_Friedel_fraction_max     0.891
_reflns_number_gt                9056
_reflns_number_total             9259
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00088a2.cif
_cod_data_source_block           d-oh-bim+bdc+zn_autored
_cod_database_code               7244727
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'Zn C H O N'
_diffrn_oxdiff_digest_frames
;
01f67c29ac4000c4668d4d84c0c8a769c501536d1f5
;
_diffrn_oxdiff_digest_hkl
;
0168f3198973b1fadfcbf1205c03b66a8eca3c
;
_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
 O66-C1
 1.35 with sigma of 0.002
3. Rigid bond restraints
 C1, O66
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C1 \\sim O66: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(C1) \\sim Ueq, Uanis(O66) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
5.a Ternary CH refined with riding coordinates:
 C49(H49), C61(H61)
5.b Aromatic/amide H refined with riding coordinates:
 N60(H60), N41(H41), C21(H21), C17(H17), C46(H46), C29(H29), C8(H8), C5(H5),
 C32(H32), C6(H6), C20(H20), C33(H33), C30(H30), C55(H55), C9(H9), C45(H45),
 C18(H18), C43(H43), C44(H44), C58(H58), C57(H57), C56(H56)
5.c Idealised Me refined as rotating group:
 C51(H51A,H51B,H51C), C63(H63A,H63B,H63C), C65(H65A,H65B,H65C)
5.d Idealised tetrahedral OH refined as rotating group:
 O50(H50), O62(H62), O64(H64), O66(H66)
;
_shelx_res_checksum              90853
_shelx_hkl_checksum              49867
_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 3.475
_oxdiff_exptl_absorpt_empirical_full_min 0.847