Nitrogen-enriched flexible metal-organic framework for CO<sub>2</sub> adsorption.
Lancheros, Andrés; Goswami, Subhadip; Zarate, Ximena; Schott, Eduardo; Hupp, Joseph T.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 14028–14036; doi:10.1039/d4dt01457j

data_7716826
_publ_section_title
;
 Nitrogen-enriched flexible metal-organic framework for CO<sub>2</sub>
 adsorption.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14028
_journal_page_last               14036
_journal_paper_doi               10.1039/d4dt01457j
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         '0.5(C192 H184 N28 O28 Zn6), 2(C3 H7 N O)'
_chemical_formula_sum            'C102 H106 N16 O16 Zn3'
_chemical_formula_weight         2008.13
_chemical_name_common            Zn3(-COO)6(DMF)2,
_chemical_name_systematic        '[Zn2(L)(DMF)]'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-02-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-05-13 deposited with the CCDC.	2024-07-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.7685(17)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.2475(3)
_cell_length_b                   10.38151(15)
_cell_length_c                   33.0497(5)
_cell_measurement_reflns_used    39860
_cell_measurement_temperature    100.01(11)
_cell_measurement_theta_max      33.8320
_cell_measurement_theta_min      2.0350
_cell_volume                     4871.48(15)
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(11)
_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 0.903
_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     -4.00  21.00   0.50   20.04    --   13.12 -37.00  60.00   50
  2  \w    -44.00 -19.00   0.50   20.04    --   13.12 -37.00  60.00   50
  3  \w    -55.00 -20.00   0.50   20.04    --   13.12 -19.00  30.00   70
  4  \w      4.00  86.00   0.50   20.04    --   13.12  77.00 -30.00  164
  5  \w    -38.00   5.00   0.50   20.04    --   13.12 -19.00-180.00   86
  6  \w      3.00  53.00   0.50   20.04    --   13.12-111.00-175.00  100
  7  \w    -52.00 -27.00   0.50   20.04    --  -13.59 111.00 -81.00   50
  8  \w    -85.00 -39.00   0.50   20.04    --  -13.59 178.00-180.00   92
  9  \w    -70.00 -39.00   0.50   20.04    --  -13.59 178.00  90.00   62
 10  \w    -84.00  -9.00   0.50   20.04    --  -13.59 -57.00 150.00  150
 11  \w    -85.00   3.00   0.50   20.04    --  -13.59 -77.00  90.00  176
 12  \w    -83.00  -6.00   0.50   20.04    --  -13.59 -57.00-120.00  154
 13  \w     48.00  73.00   0.50   20.04    --   13.12-178.00-150.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0111137000
_diffrn_orient_matrix_UB_12      -0.0417458000
_diffrn_orient_matrix_UB_13      -0.0166972000
_diffrn_orient_matrix_UB_21      0.0202078000
_diffrn_orient_matrix_UB_22      -0.0523968000
_diffrn_orient_matrix_UB_23      0.0114192000
_diffrn_orient_matrix_UB_31      -0.0443300000
_diffrn_orient_matrix_UB_32      -0.0134318000
_diffrn_orient_matrix_UB_33      0.0073710000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.903
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            112588
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.903
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.869
_diffrn_reflns_theta_min         2.057
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.807
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80115
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_description       block
_exptl_crystal_F_000             2096
_exptl_crystal_recrystallization_method
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.241
_exptl_crystal_size_mid          0.115
_exptl_crystal_size_min          0.052
_refine_diff_density_max         1.636
_refine_diff_density_min         -0.831
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     675
_refine_ls_number_reflns         17776
_refine_ls_number_restraints     180
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0879
_refine_ls_R_factor_gt           0.0652
_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^)+(0.0809P)^2^+7.1456P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1723
_refine_ls_wR_factor_ref         0.1834
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13351
_reflns_number_total             17776
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01457j2.cif
_cod_data_source_block           cx1827
_cod_depositor_comments          'Adding full bibliography for 7716826.cif.'
_cod_database_code               7716826
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         C45H42N6O6Zn
_diffrn_oxdiff_digest_frames
;
01ba2e35c2b66654617adddcec00f50306012549d84
;
_diffrn_oxdiff_digest_hkl
;
0117422150082b58124820af2d760f2b8351fc
;
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
O7 \\sim O7A \\sim N7 \\sim N7A \\sim C46 \\sim C46A \\sim C47 \\sim C47A \\sim
C48 \\sim C48A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
3. Rigid body (RIGU) restrains
 O7, O7A, N7, N7A, C46, C46A, C47, C47A, C48, C48A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Sof(O7A)=Sof(N7A)=Sof(C46A)=Sof(H46A)=Sof(C47A)=Sof(H47D)=Sof(H47E)=Sof(H47F)=
 Sof(C48A)=Sof(H48D)=Sof(H48E)=Sof(H48F)=1-FVAR(1)
 Sof(O7)=Sof(N7)=Sof(C46)=Sof(H46)=Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(H47C)=
 Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(H48C)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C20(H20A,H20B), C33(H33A,H33B)
5.b Me refined with riding coordinates:
 C47(H47A,H47B,H47C), C47A(H47D,H47E,H47F)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C15(H15), C17(H17), C19(H19), C27(H27),
 C28(H28), C30(H30), C31(H31), C40(H40), C41(H41), C43(H43), C44(H44), C46(H46),
  C46A(H46A), C49(H49)
5.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C24(H24A,H24B,H24C), C25(H25A,H25B,
 H25C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C48(H48A,H48B,H48C),
 C48A(H48D,H48E,H48F), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C)
;
_shelx_res_checksum              26489
_shelx_hkl_checksum              16186
_shelx_fab_checksum              71774
_olex2_date_sample_data_collection 2020-02-25
_olex2_date_sample_submission    2020-02-24
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a glass fibre with Paratone oil'
_olex2_submission_original_sample_id cx1827
_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 1.217
_oxdiff_exptl_absorpt_empirical_full_min 0.667