A thiourea-functionalized metal-organic macrocycle for the catalysis of Michael additions and prominent size-selective effect.
Yang, Lu; Zhao, Liang; Zhou, Zhen; He, Cheng; Sun, Hui; Duan, Chunying; Dalton transactions (Cambridge, England : 2003) 46 (2017) 4086–4092; doi:10.1039/c6dt04299f

data_7042200
_publ_section_title
;
 A thiourea-functionalized metal-organic macrocycle for the catalysis of
 Michael additions and prominent size-selective effect.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4086
_journal_page_last               4092
_journal_paper_doi               10.1039/c6dt04299f
_journal_volume                  46
_journal_year                    2017
_chemical_formula_sum            'C50 H52.5 B4 F16 N21 Ni2 O0.75 S4'
_chemical_formula_weight         1552.53
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2017-02-13 deposited with the CCDC.
2017-02-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            32
_cell_length_a                   48.447(9)
_cell_length_b                   51.450(12)
_cell_length_c                   22.862(5)
_cell_measurement_reflns_used    4873
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      18.9275
_cell_measurement_theta_min      2.198
_cell_volume                     56986(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1509
_diffrn_reflns_av_unetI/netI     0.1618
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       57
_diffrn_reflns_limit_h_min       -57
_diffrn_reflns_limit_k_max       61
_diffrn_reflns_limit_k_min       -60
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            73701
_diffrn_reflns_point_group_measured_fraction_full 0.847
_diffrn_reflns_point_group_measured_fraction_max 0.872
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.543
_exptl_absorpt_coefficient_mu    0.739
_exptl_absorpt_correction_T_max  0.8665
_exptl_absorpt_correction_T_min  0.8313
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             25264
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.860
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.100
_refine_ls_abs_structure_details
;
 Flack x determined using 2655 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.027(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.954
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1769
_refine_ls_number_reflns         21849
_refine_ls_number_restraints     1706
_refine_ls_restrained_S_all      0.953
_refine_ls_R_factor_all          0.1994
_refine_ls_R_factor_gt           0.0952
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1364P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2152
_refine_ls_wR_factor_ref         0.2550
_reflns_Friedel_coverage         0.698
_reflns_Friedel_fraction_full    0.715
_reflns_Friedel_fraction_max     0.737
_reflns_number_gt                10248
_reflns_number_total             21849
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04299f2.cif
_cod_data_source_block           Ni_PDT
_cod_depositor_comments
'Adding full bibliography for 7042200--7042201.cif.'
_cod_original_cell_volume        56986(20)
_cod_original_formula_sum        'C50 H52.50 B4 F16 N21 Ni2 O0.75 S4'
_cod_database_code               7042200
_shelx_estimated_absorpt_t_min   0.831
_shelx_estimated_absorpt_t_max   0.866
_shelxl_version_number           2014-3
_shelx_res_checksum              99153