#------------------------------------------------------------------------------
#$Date: 2024-01-12 04:40:31 +0200 (Fri, 12 Jan 2024) $
#$Revision: 289053 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/23/2312383.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2312383
loop_
_publ_author_name
'Le Garff, Paul'
'Maria Losus, Renny'
'Chaudhary, Simran'
'Dobrzańska, Liliana'
_publ_section_title
;
 Tailoring the dimensionality of metal complexes via ligand modifications.
;
_journal_issue                   1
_journal_name_full
'Acta crystallographica Section B, Structural science, crystal engineering and materials'
_journal_paper_doi               10.1107/S2052520623010260
_journal_volume                  80
_journal_year                    2024
_chemical_formula_sum            'C38 H48 Cu2 N14 O13'
_chemical_formula_weight         1035.98
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90.245(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.5524(3)
_cell_length_b                   18.5525(4)
_cell_length_c                   8.13830(10)
_cell_measurement_reflns_used    3348
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.2030
_cell_measurement_theta_min      3.8610
_cell_volume                     2197.19(7)
_computing_cell_refinement       'CrysAlisPro 1.171.42.55a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.55a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.55a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2020)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.891
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_av_unetI/netI     0.0385
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.891
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            5900
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.891
_diffrn_reflns_theta_full        67.500
_diffrn_reflns_theta_max         76.596
_diffrn_reflns_theta_min         3.861
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.890
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69137
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.55a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.566
_exptl_crystal_description       block
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.368
_refine_diff_density_min         -0.459
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         2131
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0363
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0528P)²+2.6293P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0982
_refine_ls_wR_factor_ref         0.1012
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1931
_reflns_number_total             2131
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            yv5014sup1.cif
_cod_data_source_block           5
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               2312383
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.610
_shelx_estimated_absorpt_t_max   0.928
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.500000 0.36027(2) 0.500000 0.01697(16) Uani 1 2 d S T P . .
N1 N 0.36838(12) 0.35157(9) 0.4457(2) 0.0178(4) Uani 1 1 d . . . . .
C2 C 0.29795(14) 0.37011(11) 0.5395(2) 0.0183(4) Uani 1 1 d . . . . .
H2 H 0.303351 0.392798 0.643758 0.022 Uiso 1 1 calc R U . . .
N3 N 0.21812(12) 0.35250(9) 0.4674(2) 0.0162(4) Uani 1 1 d . . . . .
C4 C 0.23800(14) 0.32033(11) 0.3189(2) 0.0185(4) Uani 1 1 d . . . . .
H4 H 0.195207 0.301853 0.241141 0.022 Uiso 1 1 calc R U . . .
C5 C 0.33095(14) 0.32038(11) 0.3062(2) 0.0200(4) Uani 1 1 d . . . . .
H5 H 0.364879 0.301970 0.215968 0.024 Uiso 1 1 calc R U . . .
C6 C 0.12530(14) 0.36393(10) 0.5358(3) 0.0172(4) Uani 1 1 d . . . . .
H6A H 0.110084 0.323731 0.610871 0.021 Uiso 1 1 calc R U . . .
H6B H 0.079634 0.363972 0.445239 0.021 Uiso 1 1 calc R U . . .
C7 C 0.11958(13) 0.43434(10) 0.6281(2) 0.0159(4) Uani 1 1 d . . . . .
C8 C 0.12063(18) 0.500000 0.5421(3) 0.0159(5) Uani 1 2 d S T P . .
C9 C 0.1129(2) 0.500000 0.8825(3) 0.0194(6) Uani 1 2 d S T P . .
H9 H 0.108658 0.500000 0.998940 0.023 Uiso 1 2 calc R U P . .
C10 C 0.11579(13) 0.43413(11) 0.8012(2) 0.0175(4) Uani 1 1 d . . . . .
C11 C 0.11859(17) 0.36554(11) 0.9006(3) 0.0244(5) Uani 1 1 d . . . . .
H11A H 0.112738 0.377165 1.017585 0.037 Uiso 1 1 calc R U . . .
H11B H 0.177102 0.340787 0.881897 0.037 Uiso 1 1 calc R U . . .
H11C H 0.067741 0.334124 0.867018 0.037 Uiso 1 1 calc R U . . .
C12 C 0.1238(2) 0.500000 0.3557(3) 0.0200(6) Uani 1 2 d S T P . .
H12A H 0.119514 0.450351 0.315237 0.030 Uiso 0.5 1 calc R U P . .
H12B H 0.181773 0.521440 0.319107 0.030 Uiso 0.5 1 calc R U P . .
H12C H 0.072192 0.528208 0.312295 0.030 Uiso 0.5 1 calc R U P . .
N13 N 0.44219(12) 0.30478(10) 0.7936(2) 0.0216(4) Uani 1 1 d . . . . .
O14 O 0.46717(10) 0.36717(8) 0.73845(17) 0.0205(3) Uani 1 1 d . . . . .
O15 O 0.46403(10) 0.25025(8) 0.71487(19) 0.0257(4) Uani 1 1 d . . . . .
O16 O 0.39698(12) 0.30241(10) 0.92138(19) 0.0351(4) Uani 1 1 d . . . . .
N17 N 0.3592(5) 0.500000 0.2543(7) 0.0367(14) Uani 0.5 2 d S T P A 1
N17A N 0.3399(4) 0.500000 -0.1827(7) 0.0294(12) Uani 0.5 2 d S T P B 2
C18 C 0.3615(7) 0.500000 0.114(2) 0.021(2) Uani 0.5 2 d S T P A 1
C19 C 0.3640(2) 0.500000 -0.0569(5) 0.0324(8) Uani 1 2 d S T P . .
C19A C 0.3915(8) 0.500000 0.121(2) 0.032(3) Uani 0.5 2 d S T P B 2
H19A H 0.408146 0.549032 0.154893 0.048 Uiso 0.5 1 calc R U P B 2
H19B H 0.444250 0.467930 0.137341 0.048 Uiso 0.5 1 calc R U P B 2
H19C H 0.339884 0.483038 0.188078 0.048 Uiso 0.5 1 calc R U P B 2
O20 O 0.5240(3) 0.500000 0.4716(5) 0.0261(10) Uiso 0.5 2 d DS . P . .
H20A H 0.562(4) 0.500000 0.574(4) 0.031 Uiso 0.5 2 d DS U P . .
H20B H 0.569(3) 0.500000 0.382(5) 0.031 Uiso 0.5 2 d DS U P . .
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'
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
N1 Cu1 N1 170.60(10) . 2_656 ?
N1 Cu1 O14 91.36(7) . 2_656 ?
N1 Cu1 O14 89.24(7) 2_656 2_656 ?
N1 Cu1 O14 89.24(7) . . ?
N1 Cu1 O14 91.36(7) 2_656 . ?
O14 Cu1 O14 172.68(8) 2_656 . ?
C2 N1 C5 106.16(17) . . ?
C2 N1 Cu1 127.07(14) . . ?
C5 N1 Cu1 126.65(14) . . ?
N1 C2 N3 110.82(18) . . ?
N1 C2 H2 124.6 . . ?
N3 C2 H2 124.6 . . ?
C2 N3 C4 107.74(17) . . ?
C2 N3 C6 126.30(17) . . ?
C4 N3 C6 125.96(17) . . ?
C5 C4 N3 106.23(17) . . ?
C5 C4 H4 126.9 . . ?
N3 C4 H4 126.9 . . ?
C4 C5 N1 109.06(17) . . ?
C4 C5 H5 125.5 . . ?
N1 C5 H5 125.5 . . ?
N3 C6 C7 111.34(16) . . ?
N3 C6 H6A 109.4 . . ?
C7 C6 H6A 109.4 . . ?
N3 C6 H6B 109.4 . . ?
C7 C6 H6B 109.4 . . ?
H6A C6 H6B 108.0 . . ?
C8 C7 C10 120.05(18) . . ?
C8 C7 C6 120.09(18) . . ?
C10 C7 C6 119.83(17) . . ?
C7 C8 C7 120.2(2) 6_565 . ?
C7 C8 C12 119.89(12) 6_565 . ?
C7 C8 C12 119.89(12) . . ?
C10 C9 C10 123.0(3) . 6_565 ?
C10 C9 H9 118.5 . . ?
C10 C9 H9 118.5 6_565 . ?
C9 C10 C7 118.32(18) . . ?
C9 C10 C11 119.13(18) . . ?
C7 C10 C11 122.50(18) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C8 C12 H12A 109.5 . . ?
C8 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C8 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C8 C12 H12A 109.47(7) . 6_565 ?
H12A C12 H12A 140.1 . 6_565 ?
H12B C12 H12A 64.6 . 6_565 ?
H12C C12 H12A 47.9 . 6_565 ?
C8 C12 H12B 109.5(4) . 6_565 ?
H12A C12 H12B 64.6 . 6_565 ?
H12B C12 H12B 47.9 . 6_565 ?
H12C C12 H12B 140.1 . 6_565 ?
H12A C12 H12B 109.5 6_565 6_565 ?
C8 C12 H12C 109.5(4) . 6_565 ?
H12A C12 H12C 47.9 . 6_565 ?
H12B C12 H12C 140.1 . 6_565 ?
H12C C12 H12C 64.6 . 6_565 ?
H12A C12 H12C 109.5 6_565 6_565 ?
H12B C12 H12C 109.5 6_565 6_565 ?
O16 N13 O15 123.05(18) . . ?
O16 N13 O14 118.43(18) . . ?
O15 N13 O14 118.51(16) . . ?
N13 O14 Cu1 110.33(11) . . ?
C18 N17 H19A 53.9(8) . 6_565 ?
N17 C18 C19 179.8(10) . . ?
N17 C18 H19A 74.8(19) . 6_565 ?
C19 C18 H19A 105(2) . 6_565 ?
N17 C18 H19B 83.7(17) . 6_565 ?
C19 C18 H19B 96.5(17) . 6_565 ?
C19 C18 H19C 145(2) . 6_565 ?
N17A C19 C19A 176.5(7) . . ?
C19 C19A H19A 109.5 . . ?
C19 C19A H19B 109.5 . . ?
H19A C19A H19B 109.5 . . ?
C19 C19A H19C 109.5 . . ?
H19A C19A H19C 109.5 . . ?
H19B C19A H19C 109.5 . . ?
C19 C19A H19A 109.5(2) . 6_565 ?
C19 C19A H19B 109.5(8) . 6_565 ?
C19 C19A H19C 109.5(6) . 6_565 ?
O20 O20 H20A 90(3) 5_666 . ?
O20 O20 H20B 165(3) 5_666 . ?
H20A O20 H20B 105(3) . . ?
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 N1 1.9704(17) . ?
Cu1 N1 1.9704(17) 2_656 ?
Cu1 O14 2.0045(14) 2_656 ?
Cu1 O14 2.0046(14) . ?
N1 C2 1.326(3) . ?
N1 C5 1.384(3) . ?
C2 N3 1.340(3) . ?
C2 H2 0.9500 . ?
N3 C4 1.379(2) . ?
N3 C6 1.478(3) . ?
C4 C5 1.357(3) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C6 C7 1.510(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.405(2) . ?
C7 C10 1.410(3) . ?
C8 C12 1.518(4) . ?
C9 C10 1.391(2) . ?
C9 C10 1.391(2) 6_565 ?
C9 H9 0.9500 . ?
C10 C11 1.508(3) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C12 H12A 0.980(3) 6_565 ?
C12 H12B 0.980(17) 6_565 ?
C12 H12C 0.98(2) 6_565 ?
N13 O16 1.233(2) . ?
N13 O15 1.240(2) . ?
N13 O14 1.294(2) . ?
N17 C18 1.142(19) . ?
C18 C19 1.392(19) . ?
C19 C19A 1.503(18) . ?
C19A H19A 0.9800 . ?
C19A H19B 0.9800 . ?
C19A H19C 0.9800 . ?
C19A H19A 0.980(11) 6_565 ?
C19A H19B 0.98(3) 6_565 ?
C19A H19C 0.98(2) 6_565 ?
O20 O20 0.840(8) 5_666 ?
O20 H20A 0.99(2) . ?
O20 H20B 0.98(2) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 N1 C2 N3 0.0(2) . . . . ?
Cu1 N1 C2 N3 -176.16(13) . . . . ?
N1 C2 N3 C4 0.4(2) . . . . ?
N1 C2 N3 C6 179.16(17) . . . . ?
C2 N3 C4 C5 -0.6(2) . . . . ?
C6 N3 C4 C5 -179.36(18) . . . . ?
N3 C4 C5 N1 0.6(2) . . . . ?
C2 N1 C5 C4 -0.3(2) . . . . ?
Cu1 N1 C5 C4 175.81(14) . . . . ?
C2 N3 C6 C7 37.6(3) . . . . ?
C4 N3 C6 C7 -143.87(19) . . . . ?
N3 C6 C7 C8 71.4(2) . . . . ?
N3 C6 C7 C10 -106.9(2) . . . . ?
C10 C7 C8 C7 1.2(4) . . . 6_565 ?
C6 C7 C8 C7 -177.07(15) . . . 6_565 ?
C10 C7 C8 C12 -179.4(2) . . . . ?
C6 C7 C8 C12 2.4(3) . . . . ?
C10 C9 C10 C7 -1.6(4) 6_565 . . . ?
C10 C9 C10 C11 175.97(19) 6_565 . . . ?
C8 C7 C10 C9 0.2(3) . . . . ?
C6 C7 C10 C9 178.4(2) . . . . ?
C8 C7 C10 C11 -177.3(2) . . . . ?
C6 C7 C10 C11 0.9(3) . . . . ?
O16 N13 O14 Cu1 -160.73(15) . . . . ?
O15 N13 O14 Cu1 18.6(2) . . . . ?

_cod_database_fobs_code 2312383
