A robust heterogeneous Co-MOF catalyst in azide‒alkyne cycloaddition and Friedel‒Crafts reactions as well as hydrosilylation of alkynes
Wu, Tai-Xue; Jia, Jun-Song; Luo, Wei; Bian, He-Dong; Tang, Hai-Tao; Pan, Ying-Ming; Huang, Fu-Ping; New Journal of Chemistry 45 (2021) 872–880; doi:10.1039/D0NJ04626D

data_7060141
_publ_section_title
;
 A robust heterogeneous Co-MOF catalyst in azide--alkyne cycloaddition and
 Friedel--Crafts reactions as well as hydrosilylation of alkynes
;
_journal_issue                   2
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              872
_journal_page_last               880
_journal_paper_doi               10.1039/D0NJ04626D
_journal_volume                  45
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C16 H13 Co2 N5 O6'
_chemical_formula_sum            'C16 H11 Co2 N5 O6'
_chemical_formula_weight         487.16
_space_group_crystal_system      hexagonal
_space_group_IT_number           173
_space_group_name_Hall           'P 6c'
_space_group_name_H-M_alt        'P 63'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-11-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-01-13 deposited with the CCDC.	2020-12-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   21.6539(6)
_cell_length_b                   21.6539(6)
_cell_length_c                   8.3373(3)
_cell_measurement_reflns_used    7850
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.2690
_cell_measurement_theta_min      3.8960
_cell_volume                     3385.54(18)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9784
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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     34.00  94.00   0.50   25.00    --   17.77-178.00 150.00  120
  2  \w    -92.00   6.00   0.50   25.00    --  -19.57 -38.00 150.00  196
  3  \w    -41.00  49.00   0.50   25.00    --  -19.57  57.00 -30.00  180
  4  \w    -26.00  43.00   0.50   25.00    --   17.77  19.00  90.00  138
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0196346000
_diffrn_orient_matrix_UB_12      -0.0331821000
_diffrn_orient_matrix_UB_13      -0.0400933000
_diffrn_orient_matrix_UB_21      0.0319507000
_diffrn_orient_matrix_UB_22      -0.0007635000
_diffrn_orient_matrix_UB_23      -0.0134075000
_diffrn_orient_matrix_UB_31      -0.0048362000
_diffrn_orient_matrix_UB_32      -0.0181271000
_diffrn_orient_matrix_UB_33      0.0738641000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_unetI/netI     0.0333
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            20859
_diffrn_reflns_point_group_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.366
_diffrn_reflns_theta_min         3.764
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.507
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61226
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_description       strip
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.214
_refine_diff_density_min         -0.228
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details
;
 Flack x determined using 1677 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.019(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         4411
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0284
_refine_ls_R_factor_gt           0.0241
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0245P)^2^+0.5763P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0563
_refine_ls_wR_factor_ref         0.0587
_reflns_Friedel_coverage         0.786
_reflns_Friedel_fraction_full    0.919
_reflns_Friedel_fraction_max     0.904
_reflns_number_gt                4054
_reflns_number_total             4411
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj04626d2.cif
_cod_data_source_block           20191122-hfp-wtx-l-co-mof-r_sq
_cod_depositor_comments
'Adding full bibliography for 7060141--7060142.cif.'
_cod_original_cell_volume        3385.5(2)
_cod_database_code               7060141
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.733
_shelx_estimated_absorpt_t_min   0.652
_reflns_odcompleteness_completeness 99.60
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 O(H,H) groups
2.a Rotating group:
 O6(H6A,H6B)
2.b Ternary CH refined with riding coordinates:
 C2(H2)
2.c Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B)
2.d Aromatic/amide H refined with riding coordinates:
 C16(H16), C14(H14), C13(H13), C15(H15), C5(H5), C8(H8), C6(H6), C7(H7)
;
_shelx_res_checksum              96223
_shelx_fab_checksum              28966
_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 1.389
_oxdiff_exptl_absorpt_empirical_full_min 0.622