A Hydrolytically Stable Cu(II)-Based Metal-Organic Framework with Easily Accessible Ligands for Water Harvesting.
Wang, Lu; Wang, Kecheng; An, Hao-Tian; Huang, Hongliang; Xie, Lin-Hua; Li, Jian-Rong; ACS applied materials & interfaces 13 (2021) 49509–49518; doi:10.1021/acsami.1c15240

data_4519084
_publ_section_title
;
 A Hydrolytically Stable Cu(II)-Based Metal-Organic Framework with Easily
 Accessible Ligands for Water Harvesting.
;
_journal_issue                   41
_journal_name_full               'ACS applied materials &amp; interfaces'
_journal_page_first              49509
_journal_page_last               49518
_journal_paper_doi               10.1021/acsami.1c15240
_journal_volume                  13
_journal_year                    2021
_chemical_formula_moiety         '0.13(C112 H96 Cu16 N80 O32), C4 H9 N O'
_chemical_formula_sum            'C18 H21 Cu2 N11 O5'
_chemical_formula_weight         598.54
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2020-03-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.7354(3)
_cell_length_b                   15.7354(3)
_cell_length_c                   22.5970(6)
_cell_measurement_reflns_used    1511
_cell_measurement_temperature    265.94(12)
_cell_measurement_theta_max      71.8150
_cell_measurement_theta_min      5.5610
_cell_volume                     5595.1(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      265.94(12)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3376
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.972
_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    -83.00  38.00   1.00    7.50    --  -42.06  19.00-150.00  121
  2  \w     20.00 110.00   1.00   15.00    --  103.05 -94.00 120.00   90
  3  \w     94.00 176.00   1.00   15.00    --  103.05 125.00  90.00   82
  4  \w     21.00 156.00   1.00   15.00    --  103.05 -15.00  90.00  135
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0407173000
_diffrn_orient_matrix_UB_12      -0.0626061000
_diffrn_orient_matrix_UB_13      0.0440940000
_diffrn_orient_matrix_UB_21      0.0750131000
_diffrn_orient_matrix_UB_22      -0.0616038000
_diffrn_orient_matrix_UB_23      -0.0088223000
_diffrn_orient_matrix_UB_31      0.0479824000
_diffrn_orient_matrix_UB_32      0.0432145000
_diffrn_orient_matrix_UB_33      0.0512484000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0648
_diffrn_reflns_av_unetI/netI     0.0631
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            7755
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.440
_diffrn_reflns_theta_min         3.423
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.287
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83995
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
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    1.421
_exptl_crystal_description       block
_exptl_crystal_F_000             2432
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.236
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         2703
_refine_ls_number_restraints     198
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0937
_refine_ls_R_factor_gt           0.0665
_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^)+(0.1065P)^2^+8.4564P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1762
_refine_ls_wR_factor_ref         0.1980
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1948
_reflns_number_total             2703
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            am1c15240_si_002.cif
_cod_data_source_block           BUT-205a
_cod_original_cell_volume        5595.1(3)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               4519084
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O N Cu'
_shelx_estimated_absorpt_t_max   0.935
_shelx_estimated_absorpt_t_min   0.914
_reflns_odcompleteness_completeness 99.02
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C8) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(N6) \\sim Ueq, Uanis(C9) \\sim
Ueq, Uanis(C10) \\sim Ueq, Uanis(C11) \\sim Ueq: with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(N3) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim
Ueq, Uanis(N4A) \\sim Ueq, Uanis(C5A) \\sim Ueq, Uanis(N3A) \\sim Ueq,
Uanis(C4A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 N2, N3, N4, C4, C5, N4A, C5A, N3A, C4A, C3, C6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C8, O3, N6, C9, C10, C11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: N3(0.5) N4(0.5) H4A(0.5) H4B(0.5) C4(0.5) H4(0.5) C5(0.5) O3(0.5)
 N6(0.5) C10(0.5) H10A(0.5) H10B(0.5) H10C(0.5) C8(0.5) C11(0.5) H11A(0.5)
 H11B(0.5) H11C(0.5) C9(0.5) H9A(0.5) H9B(0.5) H9C(0.5) N4A(0.5) H4AA(0.5)
 H4AB(0.5) C5A(0.5) N3A(0.5) C4A(0.5) H4AC(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B)
5.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C7(H7), C4A(H4AC)
5.c X=CH2 refined with riding coordinates:
 N4(H4A,H4B), N4A(H4AA,H4AB)
5.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C9(H9A,H9B,H9C)
;
_shelx_res_checksum              27888
_shelx_hkl_checksum              19802
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.208
_oxdiff_exptl_absorpt_empirical_full_min 0.875