Ideal trigonal prismatic coordination geometry of Co(II) in a honeycomb MOF with a triptycene-based ligand
Shuku, Yoshiaki; Suizu, Rie; Tsuchiizu, Masahisa; Awaga, Kunio; Chemical Communications  (2023) –; doi:10.1039/D3CC02986G

data_7131942
_publ_section_title
;
 Ideal trigonal prismatic coordination geometry of Co(II) in a honeycomb
 MOF with a triptycene-based ligand
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC02986G
_journal_year                    2023
_chemical_formula_moiety         'C20 H8 Co O6, 3(C2 H3 N)'
_chemical_formula_sum            'C26 H17 Co N3 O6'
_chemical_formula_weight         526.35
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-04-12
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-04-12 deposited with the CCDC.	2023-07-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.9411(3)
_cell_length_b                   11.4350(2)
_cell_length_c                   23.3417(4)
_cell_measurement_reflns_used    23378
_cell_measurement_temperature    123.15
_cell_measurement_theta_max      28.9980
_cell_measurement_theta_min      3.5720
_cell_volume                     5055.61(15)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      123.15
_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     64.00  90.00   0.50   20.00    --    1.30  45.00  60.00   52
  2  \w    -88.00 -37.00   0.50   20.00    --    1.30  45.00 120.00  102
  3  \w    -15.00  90.00   0.50   20.00    --    1.30  45.00 120.00  210
  4  \w    -88.00 -22.00   0.50   20.00    --    1.30  45.00  90.00  132
  5  \w     -4.00  23.00   0.50   20.00    --    1.30  45.00  90.00   54
  6  \w     43.00  90.00   0.50   20.00    --    1.30  45.00  90.00   94
  7  \w    -88.00  43.00   0.50   20.00    --    1.30  45.00  60.00  262
  8  \w    -63.00  92.00   0.50   20.00    --    2.70  45.00   0.00  310
  9  \w    -73.00  92.00   0.50   20.00    --    2.70  45.00 169.50  330
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC10 (RCD3): fixed-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0021689000
_diffrn_orient_matrix_UB_12      0.0618464000
_diffrn_orient_matrix_UB_13      0.0016254000
_diffrn_orient_matrix_UB_21      -0.0356818000
_diffrn_orient_matrix_UB_22      -0.0024304000
_diffrn_orient_matrix_UB_23      -0.0091585000
_diffrn_orient_matrix_UB_31      -0.0111720000
_diffrn_orient_matrix_UB_32      -0.0041216000
_diffrn_orient_matrix_UB_33      0.0289237000
_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  0.0372
_diffrn_reflns_av_unetI/netI     0.0107
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            150084
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         3.491
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.724
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84728
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_description       rod
_exptl_crystal_F_000             2152
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.274
_refine_diff_density_min         -0.461
_refine_diff_density_rms         0.168
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         5788
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0969
_refine_ls_R_factor_gt           0.0754
_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^)+(0.1452P)^2^+6.2619P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2452
_refine_ls_wR_factor_ref         0.2789
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3468
_reflns_number_total             5788
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc02986g2.cif
_cod_data_source_block           CoTT_revised
_cod_database_code               7131942
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CoC24H14O6N2
_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
2. Restrained distances
 C23A-C24A = C23A-C24B
 1.5 with sigma of 0.02
 C23A-N2A = C23B-N2B
 1.13 with sigma of 0.02
 C24A-N2A = C24B-N2B
 2.63 with sigma of 0.04
3. Rigid bond restraints
 C1, C3
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C1, C9
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C2, C10
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C6, C8
 with sigma for 1-2 distances of 0.0025 and sigma for 1-3 distances of 0.0025
 C11, C13
 with sigma for 1-2 distances of 0.0025 and sigma for 1-3 distances of 0.0025
 C12, C14
 with sigma for 1-2 distances of 0.0025 and sigma for 1-3 distances of 0.0025
4. Uiso/Uaniso restraints and constraints
Uanis(N2A) = Uanis(N2B)
Uanis(C23A) = Uanis(C23B)
Uanis(C24A) = Uanis(C24B)
5. Others
 Sof(N2B)=Sof(C23B)=Sof(C24B)=Sof(H24D)=Sof(H24E)=Sof(H24F)=1-FVAR(1)
 Sof(N2A)=Sof(C23A)=Sof(C24A)=Sof(H24A)=Sof(H24B)=Sof(H24C)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C1(H1), C2(H2)
6.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C11(H11), C12(H12), C17(H17), C18(H18)
6.c Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C24A(H24A,H24B,H24C), C26(H26A,H26B,H26C), C24B(H24D,
 H24E,H24F)
;
_shelx_res_checksum              59084
_shelx_hkl_checksum              73798
_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 1.245
_oxdiff_exptl_absorpt_empirical_full_min 0.883