Self-assembled mononuclear complexes: open metal sites and inverse dimension-dependent catalytic activity for Knoevenagel condensation and CO2 cycloaddition
Xu, Heng; Zhang, Le-Xi; Xing, Yue; Yin, Yanyan; Tang, Bo; Bie, Lijian; Nanoscale  (2022) –; doi:10.1039/D2NR04103K

data_1567690
_publ_section_title
;
 Self-assembled mononuclear complexes: open metal sites and inverse
 dimension-dependent catalytic activity for Knoevenagel condensation and
 CO2 cycloaddition
;
_journal_name_full               Nanoscale
_journal_paper_doi               10.1039/D2NR04103K
_journal_year                    2022
_chemical_formula_sum            'C17 H18 Cu N2 O7 S'
_chemical_formula_weight         457.93
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2021-12-26 deposited with the CCDC.	2022-09-21 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.10966(19)
_cell_length_b                   14.61582(19)
_cell_length_c                   16.4897(2)
_cell_measurement_reflns_used    7446
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      78.399
_cell_measurement_theta_min      4.918
_cell_volume                     3882.60(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_sigmaI/netI    0.0339
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16119
_diffrn_reflns_theta_full        79.50
_diffrn_reflns_theta_max         79.50
_diffrn_reflns_theta_min         4.89
_exptl_absorpt_coefficient_mu    2.978
_exptl_absorpt_correction_T_max  0.7550
_exptl_absorpt_correction_T_min  0.4686
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.567
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1880
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.626
_refine_diff_density_min         -1.579
_refine_diff_density_rms         0.129
_refine_ls_extinction_coef       0.0016(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         4151
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.252
_refine_ls_R_factor_all          0.0837
_refine_ls_R_factor_gt           0.0788
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1687P)^2^+6.5352P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2571
_refine_ls_wR_factor_ref         0.2630
_reflns_number_gt                3650
_reflns_number_total             4151
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d2nr04103k3.cif
_cod_data_source_block           Cu-TMA-22
_cod_original_cell_volume        3882.59(8)
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               1567690