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_7230060
_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         'C21 H18 F N O2 S'
_chemical_formula_sum            'C21 H18 F N O2 S'
_chemical_formula_weight         367.42
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                90.00
_cell_angle_beta                 109.925(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.4865(5)
_cell_length_b                   6.17720(10)
_cell_length_c                   15.7523(4)
_cell_measurement_reflns_used    3672
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      73.5060
_cell_measurement_theta_min      4.3980
_cell_volume                     1782.63(8)
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      294(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_details
;
  1 omega  -67.00   33.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5455   57.0000  -60.0000 100

  2 omega   -9.00   34.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5455   38.0000 -150.0000 43

  3 omega -103.00  -76.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5455  -57.0000  150.0000 27

  4 omega  -55.00  -12.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5455  -57.0000  150.0000 43

  5 omega  -83.00  -46.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5455 -167.0000  -42.0000 37

  6 omega   32.00   84.00   1.0000    1.2500
omega____ theta____ kappa____ phi______ frames
    -      107.1410  -30.0000    0.0000 52

  7 omega   48.00   89.00   1.0000    1.2500
omega____ theta____ kappa____ phi______ frames
    -      107.1410  -45.0000   90.0000 41

  8 omega   55.00   87.00   1.0000    1.2500
omega____ theta____ kappa____ phi______ frames
    -      107.1410  -95.0000   60.0000 32

  9 omega   27.00  102.00   1.0000    1.2500
omega____ theta____ kappa____ phi______ frames
    -      107.1410  -95.0000 -150.0000 75

 10 omega   37.00   88.00   1.0000    1.2500
omega____ theta____ kappa____ phi______ frames
    -      107.1410  -45.0000 -150.0000 51

 11 omega   23.00  169.00   1.0000    1.2500
omega____ theta____ kappa____ phi______ frames
    -      107.1410    0.0000 -150.0000 146
;
_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      -0.0697325000
_diffrn_orient_matrix_UB_12      0.0707715000
_diffrn_orient_matrix_UB_13      -0.0764655000
_diffrn_orient_matrix_UB_21      0.0450434000
_diffrn_orient_matrix_UB_22      0.0391385000
_diffrn_orient_matrix_UB_23      -0.0621796000
_diffrn_orient_matrix_UB_31      -0.0134232000
_diffrn_orient_matrix_UB_32      -0.2359368000
_diffrn_orient_matrix_UB_33      -0.0332125000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_unetI/netI     0.0309
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            6380
_diffrn_reflns_theta_full        73.64
_diffrn_reflns_theta_max         73.64
_diffrn_reflns_theta_min         4.83
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.828
_exptl_absorpt_correction_T_max  0.7112
_exptl_absorpt_correction_T_min  0.6578
_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    1.369
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.200
_refine_diff_density_min         -0.432
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         3487
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0492
_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^)+(0.0841P)^2^+0.1884P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1395
_refine_ls_wR_factor_ref         0.1473
_reflns_number_gt                3035
_reflns_number_total             3487
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7ra12136a2.cif
_cod_data_source_block           3ah
_cod_original_cell_volume        1782.63(7)
_cod_database_code               7230060
_chemical_oxdiff_formula         'C H O N S'
_reflns_odcompleteness_completeness 99.89
_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
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C4(H4A,H4B)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C7(H7), C8(H8), C10(H10), C12(H12), C13(H13), C14(H14), C16(H16),
 C17(H17), C19(H19), C20(H20)
2.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C)
;
_olex2_submission_special_instructions 'No special instructions were received'