#------------------------------------------------------------------------------
#$Date: 2022-09-25 02:52:24 +0300 (Sun, 25 Sep 2022) $
#$Revision: 278151 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/76/1567690.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1567690
loop_
_publ_author_name
'Xu, Heng'
'Zhang, Le-Xi'
'Xing, Yue'
'Yin, Yanyan'
'Tang, Bo'
'Bie, Lijian'
_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+0.001xFc²λ³/sin(2θ)]^-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/[σ²(Fo²)+(0.1687P)²+6.5352P] where P=(Fo²+2Fc²)/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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.01348(4) 0.78167(4) 0.14036(4) 0.0364(3) Uani 1 1 d . . .
O1 O 0.1053(2) 0.7781(2) 0.2177(2) 0.0455(8) Uani 1 1 d . . .
O3 O -0.0322(2) 0.6707(2) 0.1872(2) 0.0449(8) Uani 1 1 d . . .
S1 S 0.17623(19) 0.6677(2) -0.03806(16) 0.1021(8) Uani 1 1 d U . .
C7 C 0.0156(3) 0.6050(3) 0.2063(3) 0.0380(10) Uani 1 1 d . . .
O4 O -0.0111(2) 0.5337(3) 0.2359(3) 0.0591(11) Uani 1 1 d . . .
N1 N 0.0686(2) 0.8772(3) 0.0727(2) 0.0386(8) Uani 1 1 d . . .
N2 N -0.0486(3) 0.7632(3) 0.0362(3) 0.0454(10) Uani 1 1 d . . .
C2 C 0.1250(3) 0.6190(3) 0.1007(3) 0.0426(10) Uani 1 1 d . . .
O5 O -0.0635(2) 0.8786(3) 0.2038(3) 0.0609(11) Uani 1 1 d . . .
H5A H -0.0332 0.9119 0.2340 0.091 Uiso 1 1 d R . .
H5B H -0.0950 0.8501 0.2366 0.091 Uiso 1 1 d R . .
O2 O 0.2057(3) 0.6979(3) 0.2739(3) 0.0652(12) Uani 1 1 d . . .
C17 C 0.1274(3) 0.9349(3) 0.0985(4) 0.0493(12) Uani 1 1 d . . .
H17 H 0.1424 0.9342 0.1529 0.059 Uiso 1 1 calc R . .
C6 C 0.1425(3) 0.7037(3) 0.2313(3) 0.0404(10) Uani 1 1 d . . .
C13 C 0.0456(3) 0.8787(3) -0.0057(3) 0.0431(10) Uani 1 1 d . . .
C5 C 0.1089(3) 0.6160(3) 0.1914(3) 0.0373(9) Uani 1 1 d . . .
H5 H 0.1379 0.5631 0.2145 0.045 Uiso 1 1 calc R . .
C12 C -0.0212(3) 0.8137(4) -0.0265(3) 0.0449(11) Uani 1 1 d . . .
C16 C 0.1665(4) 0.9952(4) 0.0471(4) 0.0624(16) Uani 1 1 d . . .
H16 H 0.2070 1.0348 0.0667 0.075 Uiso 1 1 calc R . .
C4 C 0.1150(4) 0.5737(5) -0.0428(4) 0.0700(12) Uani 1 1 d DU . .
H4 H 0.0989 0.5408 -0.0885 0.084 Uiso 1 1 calc R . .
C9 C -0.1430(5) 0.6856(5) -0.0519(6) 0.080(2) Uani 1 1 d . . .
H9 H -0.1842 0.6419 -0.0593 0.096 Uiso 1 1 calc R . .
C14 C 0.0815(4) 0.9385(5) -0.0612(4) 0.0600(14) Uani 1 1 d . . .
H14 H 0.0639 0.9401 -0.1149 0.072 Uiso 1 1 calc R . .
C15 C 0.1453(5) 0.9965(5) -0.0334(5) 0.0683(17) Uani 1 1 d . . .
H15 H 0.1727 1.0351 -0.0693 0.082 Uiso 1 1 calc R . .
C1 C 0.1722(4) 0.6820(4) 0.0610(5) 0.0606(12) Uani 1 1 d U . .
H1 H 0.1998 0.7291 0.0876 0.073 Uiso 1 1 calc R . .
C8 C -0.1086(4) 0.6996(4) 0.0238(5) 0.0664(18) Uani 1 1 d . . .
H8 H -0.1269 0.6645 0.0673 0.080 Uiso 1 1 calc R . .
C3 C 0.0927(5) 0.5560(6) 0.0438(4) 0.0739(17) Uani 1 1 d DU . .
H3 H 0.0597 0.5068 0.0592 0.089 Uiso 1 1 calc R . .
C10 C -0.1150(6) 0.7379(7) -0.1166(5) 0.087(3) Uani 1 1 d . . .
H10 H -0.1369 0.7293 -0.1682 0.104 Uiso 1 1 calc R . .
C11 C -0.0539(5) 0.8032(5) -0.1035(4) 0.0692(17) Uani 1 1 d . . .
H11 H -0.0351 0.8396 -0.1460 0.083 Uiso 1 1 calc R . .
O6 O 0.1929(3) 0.0410(4) 0.2772(5) 0.102(2) Uani 1 1 d GD . .
H6A H 0.1365 0.0494 0.2779 0.15(5) Uiso 1 1 d RD . .
H6B H 0.2233 0.0998 0.2747 0.17(5) Uiso 1 1 d RD . .
O7 O 0.7745(3) 0.8781(4) 0.2263(5) 0.101(2) Uani 1 1 d D . .
H7A H 0.7507 0.8386 0.2352 0.15(5) Uiso 1 1 d RD . .
H7B H 0.7456 0.9283 0.2206 0.08(2) Uiso 1 1 d R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Cu1 O1 90.26(15) . . ?
O3 Cu1 N1 167.34(17) . . ?
O1 Cu1 N1 92.70(16) . . ?
O3 Cu1 N2 92.25(17) . . ?
O1 Cu1 N2 158.88(18) . . ?
N1 Cu1 N2 80.64(17) . . ?
O3 Cu1 O5 97.92(16) . . ?
O1 Cu1 O5 97.83(17) . . ?
N1 Cu1 O5 93.86(17) . . ?
N2 Cu1 O5 102.57(18) . . ?
C6 O1 Cu1 119.9(3) . . ?
C7 O3 Cu1 120.1(3) . . ?
C1 S1 C4 97.2(3) . . ?
O4 C7 O3 121.9(4) . . ?
O4 C7 C5 119.7(4) . . ?
O3 C7 C5 118.4(4) . . ?
C17 N1 C13 119.3(4) . . ?
C17 N1 Cu1 125.4(4) . . ?
C13 N1 Cu1 115.2(3) . . ?
C12 N2 C8 119.6(5) . . ?
C12 N2 Cu1 114.9(3) . . ?
C8 N2 Cu1 125.2(4) . . ?
C1 C2 C3 109.0(6) . . ?
C1 C2 C5 126.1(5) . . ?
C3 C2 C5 124.9(5) . . ?
N1 C17 C16 122.2(5) . . ?
O2 C6 O1 123.4(5) . . ?
O2 C6 C5 118.2(4) . . ?
O1 C6 C5 118.3(4) . . ?
N1 C13 C14 121.9(5) . . ?
N1 C13 C12 114.4(4) . . ?
C14 C13 C12 123.7(5) . . ?
C2 C5 C7 109.2(4) . . ?
C2 C5 C6 109.6(4) . . ?
C7 C5 C6 111.4(4) . . ?
N2 C12 C11 121.4(6) . . ?
N2 C12 C13 114.5(4) . . ?
C11 C12 C13 124.1(6) . . ?
C17 C16 C15 119.4(6) . . ?
C3 C4 S1 103.6(5) . . ?
C8 C9 C10 118.9(7) . . ?
C13 C14 C15 117.9(6) . . ?
C16 C15 C14 119.3(6) . . ?
C2 C1 S1 114.4(5) . . ?
N2 C8 C9 121.6(7) . . ?
C2 C3 C4 115.7(7) . . ?
C11 C10 C9 119.3(7) . . ?
C12 C11 C10 119.2(7) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O3 1.941(3) . ?
Cu1 O1 1.954(4) . ?
Cu1 N1 1.995(4) . ?
Cu1 N2 2.006(4) . ?
Cu1 O5 2.153(4) . ?
O1 C6 1.261(6) . ?
O3 C7 1.270(6) . ?
S1 C1 1.648(8) . ?
S1 C4 1.694(9) . ?
C7 O4 1.228(6) . ?
C7 C5 1.532(6) . ?
N1 C17 1.338(6) . ?
N1 C13 1.346(6) . ?
N2 C12 1.344(7) . ?
N2 C8 1.356(7) . ?
C2 C1 1.362(8) . ?
C2 C3 1.414(8) . ?
C2 C5 1.519(7) . ?
O2 C6 1.240(6) . ?
C17 C16 1.376(8) . ?
C6 C5 1.540(6) . ?
C13 C14 1.391(7) . ?
C13 C12 1.476(8) . ?
C12 C11 1.384(8) . ?
C16 C15 1.371(10) . ?
C4 C3 1.494(7) . ?
C9 C8 1.381(11) . ?
C9 C10 1.389(14) . ?
C14 C15 1.409(10) . ?
C10 C11 1.388(12) . ?
