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_7230062
_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_absolute_configuration ad
_chemical_formula_moiety         'C23 H23 N O3 S'
_chemical_formula_sum            'C23 H23 N O3 S'
_chemical_formula_weight         393.48
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.4634(2)
_cell_length_b                   9.3587(2)
_cell_length_c                   25.6617(7)
_cell_measurement_reflns_used    3141
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      73.4470
_cell_measurement_theta_min      5.0360
_cell_volume                     2032.57(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_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_details
;
  1 omega -114.00  -12.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5455  -57.0000   60.0000 102

  2 omega  -48.00  -12.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5455   38.0000 -150.0000 36

  3 omega   65.00   91.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       40.5455 -125.0000  -30.0000 26

  4 omega   70.00   96.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1410  -45.0000  -60.0000 26

  5 omega   26.00   95.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1410  -95.0000  -30.0000 69

  6 omega   51.00   78.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1410  -30.0000  150.0000 27

  7 omega   56.00  175.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1410   15.0000  120.0000 119

  8 omega   51.00   76.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1410  -30.0000 -150.0000 25
;
_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      -0.0629723000
_diffrn_orient_matrix_UB_12      0.1043621000
_diffrn_orient_matrix_UB_13      0.0415084000
_diffrn_orient_matrix_UB_21      -0.0034959000
_diffrn_orient_matrix_UB_22      0.1206450000
_diffrn_orient_matrix_UB_23      -0.0408545000
_diffrn_orient_matrix_UB_31      -0.1707756000
_diffrn_orient_matrix_UB_32      -0.0407837000
_diffrn_orient_matrix_UB_33      -0.0144732000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0134
_diffrn_reflns_av_unetI/netI     0.0216
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            5167
_diffrn_reflns_theta_full        73.57
_diffrn_reflns_theta_max         73.57
_diffrn_reflns_theta_min         3.44
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.601
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87136
_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    1.286
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.098
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.030
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.004(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         3393
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0325
_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^)+(0.0493P)^2^+0.1851P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0859
_refine_ls_wR_factor_ref         0.0885
_reflns_number_gt                3184
_reflns_number_total             3393
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7ra12136a2.cif
_cod_data_source_block           3ac
_cod_database_code               7230062
_chemical_oxdiff_formula         'C H O N S'
_chemical_oxdiff_usercomment     ZYY-2
_reflns_odcompleteness_completeness 99.81
_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), C15(H15A,H15B)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C7(H7), C8(H8), C10(H10), C11(H11), C13(H13), C14(H14), C18(H18),
 C19(H19), C21(H21), C22(H22)
2.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C23(H23A,H23B,H23C)
;
_olex2_submission_special_instructions 'No special instructions were received'