Modulation of CO<sub>2</sub> adsorption in novel pillar-layered MOFs based on carboxylate-pyrazole flexible linker.
Lancheros, Andrés; Goswami, Subhadip; Mian, Mohammad Rasel; Zhang, Xuan; Zarate, Ximena; Schott, Eduardo; Farha, Omar K.; Hupp, Joseph T.; Dalton transactions (Cambridge, England : 2003) 50 (2021) 2880–2890; doi:10.1039/d0dt03166f

data_7706531
_publ_section_title
;
 Modulation of CO<sub>2</sub> adsorption in novel pillar-layered MOFs
 based on carboxylate-pyrazole flexible linker.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2880
_journal_page_last               2890
_journal_paper_doi               10.1039/d0dt03166f
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C30 H28 N5 O4 Zn, 1[C3H7NO], 1[H2O]'
_chemical_formula_sum            'C36 H44 N7 O7 Zn'
_chemical_formula_weight         752.189
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_Int_Tables_number      12
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-10-04
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-10-07 deposited with the CCDC.	2021-01-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.598(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.3045(4)
_cell_length_b                   24.0896(6)
_cell_length_c                   14.0301(3)
_cell_measurement_reflns_used    19149
_cell_measurement_temperature    99.98(18)
_cell_measurement_theta_max      33.8340
_cell_measurement_theta_min      2.4960
_cell_volume                     6132.2(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.79a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.79a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.79a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3 (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.98(18)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.9995
_diffrn_measured_fraction_theta_max 0.8693
_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      2.00  28.00   0.50   32.00    --   13.12-100.00 170.00   52
  2  \w    -43.00 -17.00   0.50   32.00    --  -13.59 100.00 -83.00   52
  3  \w    -60.00  20.00   0.50   32.00    --   13.12 -37.00 -30.00  160
  4  \w    -22.00  45.00   0.50   32.00    --   13.12 -99.00 -60.00  134
  5  \w    -62.00   4.00   0.50   32.00    --   13.12 -19.00-150.00  132
  6  \w    -77.00  -1.00   0.50   32.00    --  -13.59 -57.00 150.00  152
  7  \w    -12.00  21.00   0.50   32.00    --  -13.59 100.00 -83.00   66
;
_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      -0.0264560000
_diffrn_orient_matrix_UB_12      -0.0201771000
_diffrn_orient_matrix_UB_13      -0.0181412000
_diffrn_orient_matrix_UB_21      0.0286797000
_diffrn_orient_matrix_UB_22      -0.0193508000
_diffrn_orient_matrix_UB_23      -0.0037728000
_diffrn_orient_matrix_UB_31      -0.0022708000
_diffrn_orient_matrix_UB_32      -0.0092539000
_diffrn_orient_matrix_UB_33      0.0475247000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_Laue_measured_fraction_full 0.9995
_diffrn_reflns_Laue_measured_fraction_max 0.8693
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            43086
_diffrn_reflns_point_group_measured_fraction_full 0.9995
_diffrn_reflns_point_group_measured_fraction_max 0.8693
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         33.82
_diffrn_reflns_theta_min         1.92
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.870
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74019
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.79a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.629
_exptl_crystal_description       plate
_exptl_crystal_F_000             3164.085
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.8913
_refine_diff_density_min         -0.7634
_refine_diff_density_rms         0.0910
_refine_ls_d_res_high            0.6385
_refine_ls_d_res_low             10.6098
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0120
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    43
_refine_ls_number_parameters     415
_refine_ls_number_reflns         10944
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0120
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0466
_refine_ls_shift/su_max          0.0009
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0726P)^2^+6.3847P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1267
_refine_ls_wR_factor_ref         0.1352
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              26
_reflns_limit_h_min              -27
_reflns_limit_k_max              36
_reflns_limit_k_min              0
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                8331
_reflns_number_total             10944
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d0dt03166f2.cif
_cod_data_source_block           20201002_ZnH2LBPY
_cod_depositor_comments
'Adding full bibliography for 7706529--7706531.cif.'
_cod_original_formula_sum        'C36 H44 N7 O7 Zn1 '
_cod_database_code               7706531
_reflns_odcompleteness_completeness 99.92
_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. Others
 Fixed Sof: C33(0.5) C34(0.5) H2(0.5) C31(0.5) C32(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C13(H13a,H13b)
3.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C3(H3), C24(H24), C20(H20), C6(H6), C4(H4), C23(H23), C21(H21),
 C29(H29), C28(H28), C26(H26), C27(H27)
3.c Idealised Me refined as rotating group:
 C12(H12a,H12b,H12c), C16(H16a,H16b,H16c), C18(H18a,H18b,H18c), C9(H9a,H9b,H9c)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 234 electrons were
found in a volume of 1018\%A^3 in 2 voids per unit cell.
This is consistent with the presence of 
1[C3H7NO], 1[H2O] per Formula Unit 
which account for 400 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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 1.179
_oxdiff_exptl_absorpt_empirical_full_min 0.795