Design and synthesis of pillared metal-organic frameworks featuring olefinic fragments.
Mander, Rachel Leigh; Schmidt, Ashley; Ruf, Michael; Korzyński, Maciej Damian; Dalton transactions (Cambridge, England : 2003) 53 (2024) 18873–18879; doi:10.1039/d4dt02397h

data_7717169
_publ_section_title
;
 Design and synthesis of pillared metal-organic frameworks featuring
 olefinic fragments.
;
_journal_issue                   47
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              18873
_journal_page_last               18879
_journal_paper_doi               10.1039/d4dt02397h
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C68 H40 N6 Ni3 O8 [+ solvent]'
_chemical_formula_sum            'C68 H40 N6 Ni3 O8'
_chemical_formula_weight         1245.19
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method
;FinalCif 2024.1-RC70 by Daniel Kratzert, Freiburg 2024, 
https://dkratzert.de/finalcif.html
;
_audit_update_record
;
2024-08-16 deposited with the CCDC.	2024-10-04 downloaded from the CCDC.
;
_cell_angle_alpha                79.613(5)
_cell_angle_beta                 83.867(5)
_cell_angle_gamma                89.992(4)
_cell_formula_units_Z            2
_cell_length_a                   16.6090(10)
_cell_length_b                   16.6570(10)
_cell_length_c                   22.4511(19)
_cell_measurement_reflns_used    9802
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      67.8403
_cell_measurement_theta_min      2.6762
_cell_measurement_wavelength     1.54178
_cell_volume                     6073.3(7)
_computing_cell_refinement       'APEX5 v2023.9-RC115 (Bruker AXS)'
_computing_data_collection       'Bruker Instrument Service v8.5.3.2 RC'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 1503)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'XT, VERSION 2018/2'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 7.391
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_details
;<Phi   scan: start= 360.0; len= 180.0; end= 540.0 at [Counterclockwise Eulerian 
angles: dx= 50.00 mm theta=  32.500 deg omega=   0.000 deg chi=  54.740 deg] 
		measure for 1.0 seconds; frame angle 1.00 degrees, wavelength=1.54184>
<Omega scan: start= 355.8; len= 118.0; end= 473.8 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=  53.829 deg phi= 240.000 deg chi=  65.500 deg] 
		measure for 15.0 seconds; frame angle 0.50 degrees, wavelength=1.54184>
<Phi   scan: start= 360.0; len=   0.5; end= 360.5 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=  46.329 deg omega=  90.699 deg chi= -44.500 deg] 
		measure for 9.0 seconds; frame angle 0.50 degrees, wavelength=1.54184>
<Phi   scan: start=   0.0; len= 360.0; end= 360.0 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=  53.829 deg omega=  11.590 deg chi=  24.000 deg] 
		measure for 15.0 seconds; frame angle 0.50 degrees, wavelength=1.54184>
<Omega scan: start= 355.8; len= 118.0; end= 473.8 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=  53.829 deg phi=  80.000 deg chi=  65.500 deg] 
		measure for 15.0 seconds; frame angle 0.50 degrees, wavelength=1.54184>
<Omega scan: start= 236.0; len= 107.5; end= 343.5 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=  -9.070 deg phi=   0.000 deg chi=  44.500 deg] 
		measure for 1.0 seconds; frame angle 0.50 degrees, wavelength=1.54184>
<Omega scan: start= 305.4; len=  94.0; end= 399.4 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta= -24.070 deg phi= 306.000 deg chi= -65.500 deg] 
		measure for 2.0 seconds; frame angle 0.50 degrees, wavelength=1.54184>
<Omega scan: start= 227.9; len= 101.0; end= 328.9 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta= -16.569 deg phi=  90.000 deg chi=  44.500 deg] 
		measure for 1.0 seconds; frame angle 0.50 degrees, wavelength=1.54184>
<Omega scan: start= 305.4; len=  94.0; end= 399.4 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta= -24.070 deg phi= 102.000 deg chi= -65.500 deg] 
		measure for 2.0 seconds; frame angle 0.50 degrees, wavelength=1.54184>
<Omega scan: start= 227.9; len= 101.0; end= 328.9 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta= -16.569 deg phi= 270.000 deg chi=  44.500 deg] 
		measure for 1.0 seconds; frame angle 0.50 degrees, wavelength=1.54184>
<Phi   scan: start= 360.0; len=   0.5; end= 360.5 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=  53.829 deg omega= 107.852 deg chi= -24.000 deg] 
		measure for 15.0 seconds; frame angle 0.50 degrees, wavelength=1.54184>
<Omega scan: start= 355.8; len= 118.0; end= 473.8 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=  53.829 deg phi= 320.000 deg chi=  65.500 deg] 
		measure for 15.0 seconds; frame angle 0.50 degrees, wavelength=1.54184>
<Omega scan: start=  75.7; len=  97.5; end= 173.2 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=  38.829 deg phi=  90.000 deg chi= -44.500 deg] 
		measure for 5.0 seconds; frame angle 0.50 degrees, wavelength=1.54184>
<Omega scan: start= 355.8; len= 118.0; end= 473.8 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=  53.829 deg phi= 160.000 deg chi=  65.500 deg] 
		measure for 15.0 seconds; frame angle 0.50 degrees, wavelength=1.54184>
<Phi   scan: start= 360.0; len=   0.5; end= 360.5 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=  38.829 deg omega=  75.699 deg chi= -44.500 deg] 
		measure for 5.0 seconds; frame angle 0.50 degrees, wavelength=1.54184>
<Omega scan: start= 355.8; len= 118.0; end= 473.8 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=  53.829 deg phi=  40.000 deg chi=  65.500 deg] 
		measure for 15.0 seconds; frame angle 0.50 degrees, wavelength=1.54184>
<Omega scan: start= 227.9; len= 101.0; end= 328.9 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta= -16.569 deg phi= 180.000 deg chi=  44.500 deg] 
		measure for 1.0 seconds; frame angle 0.50 degrees, wavelength=1.54184>
<Omega scan: start=  75.7; len=  97.5; end= 173.2 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=  38.829 deg phi= 270.000 deg chi= -44.500 deg] 
		measure for 5.0 seconds; frame angle 0.50 degrees, wavelength=1.54184>
<Omega scan: start= 355.8; len= 118.0; end= 473.8 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=  53.829 deg phi= 360.000 deg chi=  65.500 deg] 
		measure for 15.0 seconds; frame angle 0.50 degrees, wavelength=1.54184>
<Omega scan: start= 355.8; len= 118.0; end= 473.8 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=  53.829 deg phi= 200.000 deg chi=  65.500 deg] 
		measure for 15.0 seconds; frame angle 0.50 degrees, wavelength=1.54184>
<Omega scan: start= 355.8; len= 118.0; end= 473.8 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=  53.829 deg phi= 280.000 deg chi=  65.500 deg] 
		measure for 15.0 seconds; frame angle 0.50 degrees, wavelength=1.54184>
<Omega scan: start=  75.7; len=  97.5; end= 173.2 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=  38.829 deg phi= 360.000 deg chi= -44.500 deg] 
		measure for 5.0 seconds; frame angle 0.50 degrees, wavelength=1.54184>
<Omega scan: start=  75.7; len=  97.5; end= 173.2 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=  38.829 deg phi= 180.000 deg chi= -44.500 deg] 
		measure for 5.0 seconds; frame angle 0.50 degrees, wavelength=1.54184>
<Omega scan: start= 355.8; len= 118.0; end= 473.8 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=  53.829 deg phi= 120.000 deg chi=  65.500 deg] 
		measure for 15.0 seconds; frame angle 0.50 degrees, wavelength=1.54184>
<Omega scan: start= 227.9; len= 101.0; end= 328.9 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta= -16.569 deg phi=   0.000 deg chi=  44.500 deg] 
		measure for 1.0 seconds; frame angle 0.50 degrees, wavelength=1.54184>
<Omega scan: start=  90.7; len=  82.5; end= 173.2 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=  46.329 deg phi= 270.000 deg chi= -44.500 deg] 
		measure for 9.0 seconds; frame angle 0.50 degrees, wavelength=1.54184>
<Omega scan: start= 236.0; len= 107.5; end= 343.5 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=  -9.070 deg phi=  90.000 deg chi=  44.500 deg] 
		measure for 1.0 seconds; frame angle 0.50 degrees, wavelength=1.54184>
<Omega scan: start=  90.7; len=  82.5; end= 173.2 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=  46.329 deg phi=  90.000 deg chi= -44.500 deg] 
		measure for 9.0 seconds; frame angle 0.50 degrees, wavelength=1.54184>
<Omega scan: start= 305.4; len=  94.0; end= 399.4 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta= -24.070 deg phi= 204.000 deg chi= -65.500 deg] 
		measure for 2.0 seconds; frame angle 0.50 degrees, wavelength=1.54184>
<Phi   scan: start= 360.0; len=   0.5; end= 360.5 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=  53.829 deg omega= 105.699 deg chi= -44.500 deg] 
		measure for 15.0 seconds; frame angle 0.50 degrees, wavelength=1.54184>
<Omega scan: start=  90.7; len=  82.5; end= 173.2 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=  46.329 deg phi= 180.000 deg chi= -44.500 deg] 
		measure for 9.0 seconds; frame angle 0.50 degrees, wavelength=1.54184>
<Omega scan: start=  90.7; len=  82.5; end= 173.2 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=  46.329 deg phi= 360.000 deg chi= -44.500 deg] 
		measure for 9.0 seconds; frame angle 0.50 degrees, wavelength=1.54184>
<Omega scan: start= 305.4; len=  94.0; end= 399.4 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta= -24.070 deg phi=  51.000 deg chi= -65.500 deg] 
		measure for 2.0 seconds; frame angle 0.50 degrees, wavelength=1.54184>
<Omega scan: start= 236.0; len= 107.5; end= 343.5 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta=  -9.070 deg phi= 180.000 deg chi=  44.500 deg] 
		measure for 1.0 seconds; frame angle 0.50 degrees, wavelength=1.54184>
<Phi   scan: start=   0.0; len= 360.0; end= 360.0 at [Counterclockwise Eulerian 
angles: dx= 40.00 mm theta= -24.070 deg omega= 314.007 deg chi=  44.500 deg] 
		measure for 2.0 seconds; frame angle 0.50 degrees, wavelength=1.54184>
;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\F and \w scans'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1497
_diffrn_reflns_av_unetI/netI     0.0931
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            194779
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_reduction_process narrow-frame
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.27
_diffrn_reflns_theta_min         2.012
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           1.101
_diffrn_source_target            Cu
_diffrn_source_type              'I\mS 3.0'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.787
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_correction_T_min  0.937
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for single-crystal
 structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    0.681
_exptl_crystal_description       block
_exptl_crystal_F_000             1276
_exptl_crystal_size_max          0.084
_exptl_crystal_size_mid          0.073
_exptl_crystal_size_min          0.024
_refine_diff_density_max         3.419
_refine_diff_density_min         -1.355
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.828
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     706
_refine_ls_number_reflns         22313
_refine_ls_number_restraints     1144
_refine_ls_restrained_S_all      1.815
_refine_ls_R_factor_all          0.2169
_refine_ls_R_factor_gt           0.1859
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4737
_refine_ls_wR_factor_ref         0.5012
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14194
_reflns_number_total             22313
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02397h2.cif
_cod_data_source_block           cu_ni_mof_1_sq
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7717166--7717169.cif.
;
_cod_database_code               7717169
_platon_squeeze_void_probe_radius 1.20
_shelx_shelxl_version_number     2019/3
_exptl_bruker_absorpt_correction_t_ratio 0.6209
_shelx_estimated_absorpt_t_min   0.937
_shelx_estimated_absorpt_t_max   0.981
_diffrn_measurement_bruker_total_exposure_time 88757.0
_diffrn_reflns_bruker_av_norm_i  3597.958
_diffrn_reflns_bruker_number_gt  75933
_computing_bruker_data_scaling
'SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction'
_geom_details
; All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
_shelx_res_checksum              89914
_shelx_hkl_checksum              47914
_shelx_fab_checksum              96840