Two porous Ni-MOFs based on 2,4,6-tris(pyridin-4-yl)-1,3,5-triazine showing solvent determined structures and distinctive sorption properties toward CO<sub>2</sub> and alkanes.
Qian, Bin-Bin; Song, Peng-Chao; Nie, Hong-Xiang; Zhang, Bo; Zheng, Jin-Yu; Yu, Mei-Hui; Chang, Ze; Dalton transactions (Cambridge, England : 2003) 50 (2021) 5244–5250; doi:10.1039/d1dt00136a

data_7706840
_publ_section_title
;
 Two porous Ni-MOFs based on 2,4,6-tris(pyridin-4-yl)-1,3,5-triazine
 showing solvent determined structures and distinctive sorption properties
 toward CO<sub>2</sub> and alkanes.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5244
_journal_page_last               5250
_journal_paper_doi               10.1039/d1dt00136a
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety
'C30.92 H21 N4 Ni3 O17, 2[C3H7NO], 0.5[H2O], 0.5[CH4O]'
_chemical_formula_sum            'C37.42 H38 N6 Ni3 O20'
_chemical_formula_weight         1067.91
_space_group_crystal_system      trigonal
_space_group_IT_number           166
_space_group_name_Hall           '-R 3 2"'
_space_group_name_H-M_alt        'R -3 m :H'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-03-08
_audit_creation_method
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_audit_update_record
;
2021-03-08 deposited with the CCDC.	2021-03-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   27.1230(2)
_cell_length_b                   27.1230(2)
_cell_length_c                   38.1727(3)
_cell_measurement_reflns_used    18598
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      75.8350
_cell_measurement_theta_min      4.7260
_cell_volume                     24319.7(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (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  'ShelXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -38.00  34.00   0.50    5.84    --    0.00 -82.00  30.00  144
  2  \w    -37.00  -5.00   0.50    5.84    --    0.00 -82.00   0.00   64
  3  \w     94.00 185.00   0.50   23.37    --  101.30  57.00   0.00  182
  4  \w     94.00 145.00   0.50   23.37    --  101.30  19.00-180.00  102
  5  \w     94.00 191.00   0.50   23.37    --  101.30  82.00  90.00  194
  6  \w    112.00 188.00   0.50   23.37    --  101.30  82.00-150.00  152
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0374272000
_diffrn_orient_matrix_UB_12      0.0471743000
_diffrn_orient_matrix_UB_13      -0.0263021000
_diffrn_orient_matrix_UB_21      0.0484749000
_diffrn_orient_matrix_UB_22      -0.0131862000
_diffrn_orient_matrix_UB_23      0.0056303000
_diffrn_orient_matrix_UB_31      -0.0235070000
_diffrn_orient_matrix_UB_32      -0.0435828000
_diffrn_orient_matrix_UB_33      -0.0300996000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0162
_diffrn_reflns_av_unetI/netI     0.0137
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            24179
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        66.991
_diffrn_reflns_theta_max         66.991
_diffrn_reflns_theta_min         3.473
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    1.835
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83600
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_description       block
_exptl_crystal_F_000             9873
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.541
_refine_diff_density_min         -0.697
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         5146
_refine_ls_number_restraints     230
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0561
_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^)+(0.0836P)^2^+176.0993P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1578
_refine_ls_wR_factor_ref         0.1591
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4863
_reflns_number_total             5146
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00136a2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7706839--7706840.cif.'
_cod_original_cell_volume        24319.7(4)
_cod_original_sg_symbol_H-M      'R -3 m'
_cod_database_code               7706840
_shelx_shelxl_version_number     2016/6
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C21-O7
 1.5 with sigma of 0.01
3. Rigid bond restraints
 O7, C21
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C21: within 3.8A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 3.8A
O7 \\sim C21: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
5. Others
 Fixed Sof: C21(0.46) H21A(0.5) H21B(0.5) H21C(0.5)
6.a Rotating group:
 O1W(H1WA,H1WB)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C9(H9), C10(H10), C13(H13), C14(H14), C19(H19), C20(H20)
6.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 1694 electrons were 
found in a volume of 10541.6\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 2[C3H7NO], 0.5[H2O], 0.5[CH4O] per Formula Unit 
which account for 1692 electrons per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              31802
_shelx_hkl_checksum              60766
_shelx_fab_checksum              16274
_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 1.248
_oxdiff_exptl_absorpt_empirical_full_min 0.833