A high-activity cobalt-based MOF catalyst for [2 + 2 + 2] cycloaddition of diynes and alkynes: insights into alkyne affinity and selectivity control
Xu, Fen; Si, Xiao-Ju; Wang, Xiao-Ning; Kou, Hao-Dong; Chen, Di-Ming; Liu, Chun-Sen; Du, Miao; RSC Advances 8 (2018) 4895–; doi:10.1039/C7RA12136A

data_7230064
_publ_section_title
;
 A high-activity cobalt-based MOF catalyst for [2&#x00A0;+ 2 + 2]
 cycloaddition of diynes and alkynes: insights into alkyne affinity and
 selectivity control
;
_journal_issue                   9
_journal_name_full               'RSC Advances'
_journal_page_first              4895
_journal_paper_doi               10.1039/C7RA12136A
_journal_volume                  8
_journal_year                    2018
_chemical_formula_moiety         'C20 H16 Cl N O2 S'
_chemical_formula_sum            'C20 H16 Cl N O2 S'
_chemical_formula_weight         369.85
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-12-27
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-12-29 deposited with the CCDC.
2018-01-23 downloaded from the CCDC.
;
_cell_angle_alpha                88.481(2)
_cell_angle_beta                 84.657(2)
_cell_angle_gamma                89.958(2)
_cell_formula_units_Z            4
_cell_length_a                   7.5142(2)
_cell_length_b                   12.7251(4)
_cell_length_c                   18.0220(5)
_cell_measurement_reflns_used    6983
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      73.6600
_cell_measurement_theta_min      4.9200
_cell_volume                     1715.15(9)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      294(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3031
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_details
;
  1 omega  -35.00   15.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5455   38.0000  -60.0000 50

  2 omega  -48.00   33.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5455   38.0000    0.0000 81

  3 omega   39.00   81.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       40.5455  -99.0000  -30.0000 42

  4 omega   72.00   97.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       40.5455 -125.0000    0.0000 25

  5 omega   42.00   98.00   1.0000    2.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1410  -45.0000   60.0000 56

  6 omega   57.00   90.00   1.0000    2.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1410  -30.0000  -30.0000 33

  7 omega   49.00   84.00   1.0000    2.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1410  -45.0000  -30.0000 35

  8 omega   52.00  102.00   1.0000    2.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1410  -95.0000  -30.0000 50

  9 omega   90.00  120.00   1.0000    2.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1410 -125.0000  -60.0000 30

 10 omega   41.00  108.00   1.0000    2.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1410  -95.0000   90.0000 67

 11 omega   52.00  136.00   1.0000    2.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1410  -77.0000  150.0000 84

 12 omega   56.00  160.00   1.0000    2.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1410   15.0000  150.0000 104

 13 omega   94.00  131.00   1.0000    2.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1410  125.0000    0.0000 37

 14 omega   83.00  109.00   1.0000    2.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1410   45.0000    0.0000 26

 15 omega  130.00  162.00   1.0000    2.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1410   45.0000    0.0000 32

 16 omega   39.00   68.00   1.0000    2.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1410  -30.0000  -60.0000 29

 17 omega   37.00   88.00   1.0000    2.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1410  -45.0000 -120.0000 51

 18 omega   35.00   84.00   1.0000    2.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1410  -30.0000 -180.0000 49

 19 omega   32.00   90.00   1.0000    2.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1410  -30.0000  120.0000 58

 20 omega  -68.00   29.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5455   57.0000 -150.0000 97

 21 omega -111.00  -21.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5455  -57.0000   60.0000 90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0722086000
_diffrn_orient_matrix_UB_12      0.0554796000
_diffrn_orient_matrix_UB_13      0.0660098000
_diffrn_orient_matrix_UB_21      0.0292259000
_diffrn_orient_matrix_UB_22      -0.1075667000
_diffrn_orient_matrix_UB_23      0.0381914000
_diffrn_orient_matrix_UB_31      0.1906102000
_diffrn_orient_matrix_UB_32      -0.0042970000
_diffrn_orient_matrix_UB_33      -0.0395026000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_unetI/netI     0.0429
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            11482
_diffrn_reflns_theta_full        73.78
_diffrn_reflns_theta_max         73.78
_diffrn_reflns_theta_min         3.47
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.218
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57132
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.248
_refine_diff_density_min         -0.616
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         6691
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0465
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0716P)^2^+0.2538P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1196
_refine_ls_wR_factor_ref         0.1257
_reflns_number_gt                5953
_reflns_number_total             6691
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7ra12136a2.cif
_cod_data_source_block           3ba
_cod_database_code               7230064
_chemical_oxdiff_formula         'C H O N S'
_chemical_oxdiff_usercomment     1-95
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C4(H4A,H4B), C21(H21A,H21B), C24(H24A,H24B)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C7(H7), C8(H8), C10(H10), C11(H11), C12(H12), C13(H13), C14(H14),
 C16(H16), C17(H17), C18(H18), C19(H19), C25(H25), C27(H27), C28(H28), C30(H30),
  C31(H31), C32(H32), C33(H33), C34(H34), C36(H36), C37(H37), C38(H38), C39(H39)
;
_olex2_submission_special_instructions 'No special instructions were received'