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_7706529
_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 H26 Cu N5 O4'
_chemical_formula_sum            'C30 H26 Cu N5 O4'
_chemical_formula_weight         584.10
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-03-24
_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                 97.387(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.1598(14)
_cell_length_b                   24.203(2)
_cell_length_c                   13.9450(11)
_cell_measurement_reflns_used    9840
_cell_measurement_temperature    100.02
_cell_measurement_theta_max      28.47
_cell_measurement_theta_min      2.24
_cell_volume                     6078.3(8)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.02
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_unetI/netI     0.0393
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            60389
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.100
_diffrn_reflns_theta_min         1.409
_exptl_absorpt_coefficient_mu    0.759
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.7008
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0824 before and 0.0463 after correction.
The Ratio of minimum to maximum transmission is 0.9394.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear greenish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_description       plate
_exptl_crystal_F_000             2416
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.951
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         9118
_refine_ls_number_restraints     75
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0842
_refine_ls_R_factor_gt           0.0555
_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^)+(0.0802P)^2^+10.6110P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1492
_refine_ls_wR_factor_ref         0.1641
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6297
_reflns_number_total             9118
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03166f2.cif
_cod_data_source_block           20200304cu_andres_0m
_cod_depositor_comments
'Adding full bibliography for 7706529--7706531.cif.'
_cod_original_cell_volume        6078.4(8)
_cod_database_code               7706529
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.963
_shelx_estimated_absorpt_t_min   0.863
_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. Restrained planarity
 C28, C29, C30, N5, C26, C27
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
N6 \\sim C34 \\sim C35 \\sim C31 \\sim C32 \\sim C33: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
C28 \\sim C29 \\sim C30 \\sim N5 \\sim C26 \\sim C27: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 N5, C28
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C29(0.5) H29(0.5) C30(0.5) H30(0.5) C26(0.5) H26(0.5) C27(0.5)
 H27(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B)
6.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C24(H24), C3(H3), C23(H23), C21(H21), C4(H4), C20(H20), C6(H6),
 C33(H33), C32(H32), C35(H35), C34(H34), C29(H29), C30(H30), C26(H26), C27(H27)
6.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C9(H9A,H9B,H9C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_smtbx_masks_special_details
;
A solvent mask was calculated and two voids of 
104.5 electrons, in a volume of 476.7\%A^3 each, were found per unit cell. This is 
consistent with the presence of 0.5[C3H7NO] and 0.5[H2O]per Formula 
Unit.
;