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_7706530
_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         'C31 H36 Cu N6 O4'
_chemical_formula_sum            'C31 H36 Cu N6 O4'
_chemical_formula_weight         620.20
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-03-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-10-07 deposited with the CCDC.	2021-01-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.233(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.3159(2)
_cell_length_b                   26.0056(4)
_cell_length_c                   13.1078(2)
_cell_measurement_reflns_used    8498
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      72.5180
_cell_measurement_theta_min      3.4170
_cell_volume                     3114.73(10)
_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(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.962
_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    -19.00  26.00   0.50   15.00    --  -48.45  19.00 -60.00   90
  2  \w    -57.00 -28.00   0.50   60.00    --  -98.15  57.00  90.00   58
  3  \w   -127.00-101.00   0.50   60.00    --  -98.15 -37.00  30.00   52
  4  \w   -119.00 -91.00   0.50   15.00    --  -48.45-125.00 -90.00   56
  5  \w   -100.00 -52.00   0.50   15.00    --  -48.45-157.00 -15.00   96
  6  \w   -109.00 -53.00   0.50   60.00    --  -98.15-157.00 -15.00  112
  7  \w   -166.00-134.00   0.50   60.00    --  -98.15 -37.00  30.00   64
  8  \w    -56.00 -26.00   0.50   60.00    --  -98.15  57.00-120.00   60
  9  \w    -87.00 -50.00   0.50   15.00    --  -48.45 118.00-135.00   74
 10  \w     55.00 118.00   0.50   15.00    --   50.32 157.00  18.00  126
 11  \w     82.00 107.00   0.50   60.00    --  100.03 157.00  18.00   50
 12  \w    110.00 171.00   0.50   60.00    --  100.03   0.00 -30.00  122
 13  \w     68.00 107.00   0.50   60.00    --  100.03-118.00 138.00   78
 14  \w     27.00  52.00   0.50   15.00    --   50.32-118.00 138.00   50
 15  \w     34.00  62.00   0.50   60.00    --  100.03 -57.00 150.00   56
 16  \w     28.00 105.00   0.50   60.00    --  100.03 -99.00 150.00  154
 17  \w     28.00  54.00   0.50   60.00    --  100.03 -99.00   0.00   52
 18  \w     28.00  64.00   0.50   60.00    --  100.03 -57.00  30.00   72
 19  \w     39.00  64.00   0.50   60.00    --  100.03 -57.00 -30.00   50
 20  \w     33.00  59.00   0.50   60.00    --  100.03 -57.00   0.00   52
 21  \w    -15.00  13.00   0.50   15.00    --   50.32 -19.00-150.00   56
 22  \w     29.00  64.00   0.50   60.00    --  100.03 -57.00-150.00   70
 23  \w     32.00  64.00   0.50   60.00    --  100.03 -57.00-180.00   64
 24  \w    -20.00  11.00   0.50   15.00    --   50.32 -19.00 120.00   62
 25  \w   -108.00 -44.00   0.50   60.00    --  -98.15 118.00-135.00  128
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0209389000
_diffrn_orient_matrix_UB_12      -0.0587012000
_diffrn_orient_matrix_UB_13      0.0091944000
_diffrn_orient_matrix_UB_21      -0.0932917000
_diffrn_orient_matrix_UB_22      -0.0014519000
_diffrn_orient_matrix_UB_23      0.0849547000
_diffrn_orient_matrix_UB_31      -0.1387739000
_diffrn_orient_matrix_UB_32      -0.0078883000
_diffrn_orient_matrix_UB_33      -0.0840522000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0488
_diffrn_reflns_av_unetI/netI     0.0444
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21276
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.355
_diffrn_reflns_theta_min         3.399
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.353
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.895
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
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    1.323
_exptl_crystal_description       plate
_exptl_crystal_F_000             1300
_exptl_crystal_recrystallization_method
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.112
_exptl_crystal_size_mid          0.073
_exptl_crystal_size_min          0.028
_refine_diff_density_max         0.649
_refine_diff_density_min         -0.665
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         6032
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0521
_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^)+(0.0542P)^2^+4.7157P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1301
_refine_ls_wR_factor_ref         0.1376
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5179
_reflns_number_total             6032
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03166f2.cif
_cod_data_source_block           cx1829
_cod_depositor_comments
'Adding full bibliography for 7706529--7706531.cif.'
_cod_database_code               7706530
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         C45H42N6O6
_diffrn_oxdiff_digest_frames
;
01ae663c5d50efd785757cbe05667eee96000257633
;
_diffrn_oxdiff_digest_hkl
;
013e8c9780fb6cd466be6b86b9087a8c18c0e1
;
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.99
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H13A,H13B} of C13, {H31A,H31B} of C31, {H30A,H30B} of C30,
   {H28A,H28B} of C28, {H29A,H29B} of C29, {H26A,H26B} of C26, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, {H27A,H27B} of C27
2.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C26(H26A,H26B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,
 H30B), C31(H31A,H31B)
2.b Aromatic/amide H refined with riding coordinates:
 N2(H2), N4(H4), C3(H3), C4(H4A), C6(H6), C7(H7), C20(H20), C21(H21), C23(H23),
  C24(H24)
2.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C)
;
_shelx_res_checksum              83196
_shelx_hkl_checksum              86102
_shelx_fab_checksum              32271
_olex2_date_sample_data_collection 2020-02-28
_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 MITIGEN holder'
_olex2_submission_original_sample_id cx1829
_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 2.080
_oxdiff_exptl_absorpt_empirical_full_min 0.471