#------------------------------------------------------------------------------
#$Date: 2024-12-06 22:25:12 +0200 (Fri, 06 Dec 2024) $
#$Revision: 296655 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/06/34/7063489.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_7063489
loop_
_publ_author_name
'Panda, Subhashree S.'
'Kumari, Supriya'
'Dixit, Manjusha'
'Sharma, Nagendra K.'
_publ_section_title
;
 Synthesis and DNA cleavage studies of rationally designed metallopeptides
 from N-salicyl-AA-picolamide (SAP) and Cu(ii) ions
;
_journal_issue                   45
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              19188
_journal_page_last               19194
_journal_paper_doi               10.1039/D4NJ03573A
_journal_volume                  48
_journal_year                    2024
_chemical_formula_moiety         'C15 H13 Cu N3 O3'
_chemical_formula_sum            'C15 H13 Cu N3 O3'
_chemical_formula_weight         346.83
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     direct
_audit_creation_date             2022-12-02
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2024-01-20 deposited with the CCDC.	2024-10-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.164(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.3112(9)
_cell_length_b                   6.6485(5)
_cell_length_c                   18.4942(14)
_cell_measurement_reflns_used    6089
_cell_measurement_temperature    297.3(9)
_cell_measurement_theta_max      30.5290
_cell_measurement_theta_min      3.6820
_cell_volume                     1348.53(19)
_computing_cell_refinement       'CrysAlisPro 1.171.42.52a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.52a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.52a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      297.15
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.9967
_diffrn_measured_fraction_theta_max 0.9967
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -1.00  49.00   0.50   36.68    --    3.51-116.00  27.00  100
  2  ω    -60.00   3.00   0.50   36.68    --    3.51 -37.00  60.00  126
  3  ω      7.00  39.00   0.50   36.68    --    3.51  37.00-150.00   64
  4  ω    -42.00   7.00   0.50   36.68    --    3.51 -77.00-120.00   98
  5  ω    -15.00  17.00   0.50   36.68    --   -4.14  77.00  60.00   64
  6  ω    -15.00  17.00   0.50   36.68    --   -4.14 -99.00 -30.00   64
  7  ω    -27.00   9.00   0.50   36.68    --   -4.14  77.00 150.00   72
  8  ω      5.00  31.00   0.50   36.68    --   -4.14 -99.00-150.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Dual, Cu at home/near, Pilatus 200K'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0586
_diffrn_reflns_av_unetI/netI     0.0488
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            12828
_diffrn_reflns_theta_full        26.3650
_diffrn_reflns_theta_max         26.36
_diffrn_reflns_theta_min         3.58
_exptl_absorpt_coefficient_mu    1.636
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64509
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.52a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orangish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.7082
_exptl_crystal_description       needle
_exptl_crystal_F_000             709.6318
_exptl_crystal_preparation       'As per the reaction scheme'
_exptl_crystal_recrystallization_method 'Slow evaporation'
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.3668
_refine_diff_density_min         -0.3477
_refine_diff_density_rms         0.0801
_refine_ls_d_res_high            0.8002
_refine_ls_d_res_low             5.6854
_refine_ls_goodness_of_fit_ref   1.0286
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    24
_refine_ls_number_parameters     200
_refine_ls_number_reflns         2748
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0286
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0319
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0301P)²+0.8084P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0783
_refine_ls_wR_factor_ref         0.0814
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              13
_reflns_limit_h_min              -14
_reflns_limit_k_max              8
_reflns_limit_k_min              0
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                2378
_reflns_number_total             2748
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4nj03573a2.cif
_cod_data_source_block           NKS-SSDP-221-Cu_auto
_cod_depositor_comments
'Adding full bibliography for 7063489--7063491.cif.'
_cod_database_code               7063489
_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 O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C10(H10a,H10b), C8(H8a,H8b)
2.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C5(H5), C2(H2), C12(H12), C14(H14), C3(H3), C4(H4), C13(H13)
2.c Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_olex2_exptl_crystal_mounting_method 'mMethod on the loop'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,y+1/2,-z+1/2
3 -x,-y,-z
4 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_refinement_flags_posn
Cu1 Cu 0.71528(2) 0.40739(4) 0.589905(14) 0.02752(11) Uani 1.000000 .
O3 O 0.45044(15) 0.7044(3) 0.65349(9) 0.0382(4) Uani 1.000000 .
O2 O 0.83407(15) 0.2178(3) 0.58515(9) 0.0373(4) Uani 1.000000 .
O1 O 0.67759(18) 0.0611(3) 0.76780(11) 0.0493(5) Uani 1.000000 .
H1 H 0.637(3) 0.147(2) 0.7825(12) 0.0740(8) Uiso 1.000000 GR
N3 N 0.73902(17) 0.5809(3) 0.50644(10) 0.0287(4) Uani 1.000000 .
N2 N 0.59063(17) 0.5989(3) 0.59108(10) 0.0295(4) Uani 1.000000 .
N1 N 0.66160(16) 0.2849(3) 0.67115(10) 0.0299(4) Uani 1.000000 .
C11 C 0.66867(19) 0.7455(4) 0.49369(11) 0.0273(5) Uani 1.000000 .
C9 C 0.53157(19) 0.5834(3) 0.64317(12) 0.0284(5) Uani 1.000000 .
C1 C 0.8548(2) 0.0531(4) 0.62571(12) 0.0278(5) Uani 1.000000 .
C6 C 0.79788(19) -0.0001(4) 0.68386(11) 0.0268(5) Uani 1.000000 .
C10 C 0.57475(19) 0.7649(4) 0.53936(12) 0.0287(5) Uani 1.000000 .
H10a H 0.49322(19) 0.7623(4) 0.50685(12) 0.0344(6) Uiso 1.000000 R
H10b H 0.58560(19) 0.8914(4) 0.56632(12) 0.0344(6) Uiso 1.000000 R
C7 C 0.7068(2) 0.1260(4) 0.70769(12) 0.0290(5) Uani 1.000000 .
C15 C 0.8274(2) 0.5561(4) 0.46977(13) 0.0349(5) Uani 1.000000 .
H15 H 0.8756(2) 0.4411(4) 0.47854(13) 0.0419(6) Uiso 1.000000 R
C8 C 0.5682(2) 0.4043(4) 0.69457(13) 0.0325(5) Uani 1.000000 .
H8a H 0.4972(2) 0.3212(4) 0.69337(13) 0.0390(6) Uiso 1.000000 R
H8b H 0.5998(2) 0.4508(4) 0.74534(13) 0.0390(6) Uiso 1.000000 R
C5 C 0.8300(2) -0.1845(4) 0.72116(13) 0.0336(5) Uani 1.000000 .
H5 H 0.7912(2) -0.2217(4) 0.75802(13) 0.0403(6) Uiso 1.000000 R
C2 C 0.9432(2) -0.0812(4) 0.61118(13) 0.0342(5) Uani 1.000000 .
H2 H 0.9819(2) -0.0491(4) 0.57375(13) 0.0410(6) Uiso 1.000000 R
C12 C 0.6833(2) 0.8888(4) 0.44249(13) 0.0358(6) Uani 1.000000 .
H12 H 0.6323(2) 1.0004(4) 0.43298(13) 0.0430(7) Uiso 1.000000 R
C14 C 0.8482(2) 0.6970(4) 0.41965(13) 0.0392(6) Uani 1.000000 .
H14 H 0.9108(2) 0.6794(4) 0.39572(13) 0.0470(7) Uiso 1.000000 R
C3 C 0.9738(2) -0.2555(4) 0.64985(14) 0.0392(6) Uani 1.000000 .
H3 H 1.0337(2) -0.3381(4) 0.63916(14) 0.0471(7) Uiso 1.000000 R
C4 C 0.9160(2) -0.3115(4) 0.70546(14) 0.0388(6) Uani 1.000000 .
H4 H 0.9354(2) -0.4320(4) 0.73120(14) 0.0466(7) Uiso 1.000000 R
C13 C 0.7745(2) 0.8640(4) 0.40569(13) 0.0397(6) Uani 1.000000 .
H13 H 0.7863(2) 0.9600(4) 0.37153(13) 0.0476(7) Uiso 1.000000 R
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.0030380000826
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
C 0.00347 0.00161 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.215599998832
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Cu 0.34125 1.28947 13.33800 7.16760 5.61580 1.67350 3.58280 0.24700 11.39660
64.81260 1.19099998474
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
O 0.01158 0.00611 3.04850 2.28680 1.54630 0.86700 13.27710 5.70110 0.32390
32.90890 0.250800013542
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
N 0.00653 0.00323 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.5290002823
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
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
N3 Cu1 O2 96.86(7) . . ?
N2 Cu1 O2 177.88(8) . . ?
N2 Cu1 N3 82.10(7) . . ?
N1 Cu1 O2 96.85(7) . . ?
N1 Cu1 N3 166.28(8) . . ?
N1 Cu1 N2 84.18(8) . . ?
C1 O2 Cu1 124.53(13) . . ?
C11 N3 Cu1 114.93(14) . . ?
C15 N3 Cu1 125.08(16) . . ?
C15 N3 C11 119.52(19) . . ?
C9 N2 Cu1 118.06(16) . . ?
C10 N2 Cu1 118.45(13) . . ?
C10 N2 C9 123.17(19) . . ?
C7 N1 Cu1 126.32(15) . . ?
C8 N1 Cu1 112.76(14) . . ?
C8 N1 C7 120.64(18) . . ?
C10 C11 N3 116.01(19) . . ?
C12 C11 N3 121.23(19) . . ?
C12 C11 C10 122.7(2) . . ?
N2 C9 O3 125.5(2) . . ?
C8 C9 O3 119.98(19) . . ?
C8 C9 N2 114.48(19) . . ?
C6 C1 O2 125.9(2) . . ?
C2 C1 O2 116.90(19) . . ?
C2 C1 C6 117.2(2) . . ?
C7 C6 C1 124.1(2) . . ?
C5 C6 C1 118.3(2) . . ?
C5 C6 C7 117.56(19) . . ?
C11 C10 N2 108.29(18) . . ?
N1 C7 O1 124.4(2) . . ?
C6 C7 O1 114.0(2) . . ?
C6 C7 N1 121.63(19) . . ?
C14 C15 N3 121.6(2) . . ?
C9 C8 N1 110.19(17) . . ?
C4 C5 C6 122.9(2) . . ?
C3 C2 C1 122.6(2) . . ?
C13 C12 C11 119.1(2) . . ?
C13 C14 C15 118.7(2) . . ?
C4 C3 C2 120.6(2) . . ?
C3 C4 C5 118.4(2) . . ?
C14 C13 C12 119.8(2) . . ?
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 O2 1.8601(16) . ?
Cu1 N3 1.9969(18) . ?
Cu1 N2 1.9039(18) . ?
Cu1 N1 1.9329(17) . ?
O3 C9 1.269(3) . ?
O2 C1 1.315(3) . ?
O1 C7 1.308(3) . ?
N3 C11 1.340(3) . ?
N3 C15 1.349(3) . ?
N2 C9 1.304(3) . ?
N2 C10 1.443(3) . ?
N1 C7 1.291(3) . ?
N1 C8 1.469(3) . ?
C11 C10 1.516(3) . ?
C11 C12 1.381(3) . ?
C9 C8 1.517(3) . ?
C1 C6 1.426(3) . ?
C1 C2 1.415(3) . ?
C6 C7 1.476(3) . ?
C6 C5 1.411(3) . ?
C15 C14 1.377(3) . ?
C5 C4 1.372(3) . ?
C2 C3 1.362(3) . ?
C12 C13 1.378(3) . ?
C14 C13 1.374(4) . ?
C3 C4 1.397(4) . ?
