A terpyridine-based copper complex for electrochemical reduction of nitrite to nitric oxide.
Biswas, Jyotiprokash; Sanden, Sebastian; Bhardwaj, Prabhakar; Siegmund, Daniel; Kumar, Pankaj; Apfel, Ulf-Peter; Dalton transactions (Cambridge, England : 2003) 54 (2025) 1815–1826; doi:10.1039/d4dt02777a

data_7717639
_publ_section_title
;
 A terpyridine-based copper complex for electrochemical reduction of
 nitrite to nitric oxide.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1815
_journal_page_last               1826
_journal_paper_doi               10.1039/d4dt02777a
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C15 H11 Cu N4 O2, Cl O4, C2 H3 N'
_chemical_formula_sum            'C17 H14 Cl Cu N5 O6'
_chemical_formula_weight         483.32
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-08-06
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-08-11 deposited with the CCDC.	2024-12-04 downloaded from the CCDC.
;
_cell_angle_alpha                79.875(4)
_cell_angle_beta                 78.508(4)
_cell_angle_gamma                73.768(4)
_cell_formula_units_Z            2
_cell_length_a                   7.7304(4)
_cell_length_b                   10.1821(5)
_cell_length_c                   12.9851(7)
_cell_measurement_reflns_used    6195
_cell_measurement_temperature    104.2(7)
_cell_measurement_theta_max      76.5740
_cell_measurement_theta_min      3.4980
_cell_volume                     953.80(9)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      104.2(7)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.905
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     29.00  80.00   0.50    0.22    --   47.31  67.00 133.00  102
  2  \w     88.00 113.00   0.50    0.22    --   47.31  67.00 133.00   50
  3  \w    136.00 161.00   0.50    0.87    --  105.88  67.00 133.00   50
  4  \w    147.00 173.00   0.50    0.87    --  105.88  15.00  60.00   52
  5  \w    115.00 141.00   0.50    0.87    --  105.88  15.00  60.00   52
  6  \w     26.00  63.00   0.50    0.22    --   47.31 -67.00  -0.00   74
  7  \w    -23.00   7.00   0.50    0.22    --   47.31 -67.00  -0.00   60
  8  \w    -19.00  24.00   0.50    0.22    --   47.31 -19.00   0.00   86
  9  \w    -22.00   3.00   0.50    0.22    --   47.31 -19.00-120.00   50
 10  \w     78.00 103.00   0.50    0.87    --  105.88-125.00   0.00   50
 11  \w     70.00 104.00   0.50    0.87    --  105.88 -94.00 120.00   68
 12  \w     36.00  63.00   0.50    0.87    --  105.88 -94.00 120.00   54
 13  \w     34.00  59.00   0.50    0.87    --  105.88 -94.00  60.00   50
 14  \w     63.00 103.00   0.50    0.87    --  105.88 -94.00  60.00   80
 15  \w     43.00  68.00   0.50    0.87    --  105.88-125.00   0.00   50
 16  \w     68.00 106.00   0.50    0.87    --  105.88 -94.00 -30.00   76
 17  \w     79.00 104.00   0.50    0.87    --  105.88 -94.00 -90.00   50
 18  \w     51.00  95.00   0.50    0.87    --  105.88 -94.00-120.00   88
 19  \w     34.00  67.00   0.50    0.87    --  105.88 -94.00-180.00   66
 20  \w     71.00 105.00   0.50    0.87    --  105.88 -94.00-180.00   68
 21  \w     74.00  99.00   0.50    0.87    --  105.88 -94.00-150.00   50
 22  \w     36.00  65.00   0.50    0.87    --  105.88 -67.00  -0.00   58
 23  \w     43.00  70.00   0.50    0.87    --  105.88 -61.00  30.00   54
 24  \w     46.00  71.00   0.50    0.87    --  105.88 -61.00 150.00   50
 25  \w    -58.00 -30.00   0.50    0.22    --  -47.31  67.00 133.00   56
 26  \w    -15.00  11.00   0.50    0.22    --  -47.31  67.00 133.00   52
 27  \w    -66.00 -23.00   0.50    0.87    --  -90.00  67.00 133.00   86
 28  \w    -65.00 -21.00   0.50    0.87    --  -90.00  61.00 -30.00   88
 29  \w    -48.00 -20.00   0.50    0.87    --  -90.00  45.00 -30.00   56
 30  \w    -47.00 -19.00   0.50    0.87    --  -90.00  45.00 -60.00   56
 31  \w    -47.00 -18.00   0.50    0.87    --  -90.00  45.00-120.00   58
 32  \w   -116.00 -89.00   0.50    0.22    --  -47.31 -67.00  -0.00   54
 33  \w    -74.00 -33.00   0.50    0.22    --  -47.31 -67.00  -0.00   82
 34  \w   -109.00 -72.00   0.50    0.87    --  -90.00 -67.00  -0.00   74
 35  \w   -160.00-114.00   0.50    0.87    --  -90.00 -67.00  -0.00   92
 36  \w   -162.00 -88.00   0.50    0.87    --  -90.00 -30.00  60.00  148
 37  \w   -162.00 -76.00   0.50    0.87    --  -90.00 -15.00 120.00  172
 38  \w    -45.00 -19.00   0.50    0.87    --  -90.00 125.00  60.00   52
 39  \w   -119.00 -78.00   0.50    0.87    --  -90.00 -30.00-150.00   82
 40  \w   -162.00-137.00   0.50    0.87    --  -90.00 -30.00-150.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0377648000
_diffrn_orient_matrix_UB_12      -0.1562372000
_diffrn_orient_matrix_UB_13      0.0368554000
_diffrn_orient_matrix_UB_21      -0.1716315000
_diffrn_orient_matrix_UB_22      0.0248416000
_diffrn_orient_matrix_UB_23      0.0851628000
_diffrn_orient_matrix_UB_31      -0.1153788000
_diffrn_orient_matrix_UB_32      -0.0147154000
_diffrn_orient_matrix_UB_33      -0.0793039000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.905
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9294
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.905
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.599
_diffrn_reflns_theta_min         3.502
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.342
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49457
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.683
_exptl_crystal_description       prism
_exptl_crystal_F_000             490
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.412
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         3631
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0340
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0475P)^2^+0.5647P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0858
_refine_ls_wR_factor_ref         0.0874
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3357
_reflns_number_total             3631
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02777a2.cif
_cod_data_source_block           jp271
_cod_depositor_comments
'Adding full bibliography for 7717638--7717643.cif.'
_cod_database_code               7717639
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         'C15 H11 N4 Cu Cl O6'
_shelx_estimated_absorpt_t_max   0.731
_shelx_estimated_absorpt_t_min   0.617
_reflns_odcompleteness_completeness 98.33
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C12(H12), C13(H13),
 C14(H14), C15(H15)
1.b Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C)
;
_shelx_res_checksum              69844
_shelx_hkl_checksum              27213
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 2.237
_oxdiff_exptl_absorpt_empirical_full_min 0.532