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_7717640
_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         'C17 H14 Cu N4, 2(Cl O4)'
_chemical_formula_sum            'C17 H14 Cl2 Cu N4 O8'
_chemical_formula_weight         536.76
_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                98.785(3)
_cell_angle_beta                 97.177(3)
_cell_angle_gamma                97.049(3)
_cell_formula_units_Z            4
_cell_length_a                   8.6165(4)
_cell_length_b                   8.6728(4)
_cell_length_c                   27.0547(8)
_cell_measurement_reflns_used    10342
_cell_measurement_temperature    105.4(9)
_cell_measurement_theta_max      76.8560
_cell_measurement_theta_min      3.2920
_cell_volume                     1961.56(14)
_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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      105.4(9)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.892
_diffrn_measured_fraction_theta_max 0.820
_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    -81.00  -2.00   0.50    1.09    --  -46.94 109.00 152.00  158
  2  \w     30.00  55.00   0.50    1.09    --   46.94-109.00  56.00   50
  3  \w   -146.00-121.00   0.50    4.35    --  -90.00-109.00  56.00   50
  4  \w    -74.00 -49.00   0.50    4.35    --  -90.00 109.00 152.00   50
  5  \w    107.00 163.00   0.50    4.35    --  105.88 109.00 152.00  112
  6  \w     70.00 105.00   0.50    4.35    --  105.88-109.00  56.00   70
  7  \w   -108.00 -82.00   0.50    1.09    --  -46.94-125.00-120.00   52
  8  \w   -115.00 -85.00   0.50    1.09    --  -46.94-125.00  90.00   60
  9  \w    -22.00  24.00   0.50    1.09    --  -46.94  19.00  90.00   92
 10  \w   -116.00 -75.00   0.50    1.09    --  -46.94-125.00-150.00   82
 11  \w    -23.00   5.00   0.50    1.09    --  -46.94  19.00   0.00   56
 12  \w    -47.00 -21.00   0.50    4.35    --  -90.00  45.00 -30.00   52
 13  \w    -48.00 -19.00   0.50    4.35    --  -90.00  45.00 -90.00   58
 14  \w    -77.00 -50.00   0.50    4.35    --  -90.00 125.00-180.00   54
 15  \w    -48.00 -18.00   0.50    4.35    --  -90.00  45.00 150.00   60
 16  \w   -164.00 -78.00   0.50    4.35    --  -90.00 -30.00 150.00  172
 17  \w    -48.00 -18.00   0.50    4.35    --  -90.00  45.00   0.00   60
 18  \w    -47.00 -21.00   0.50    4.35    --  -90.00  45.00-180.00   52
 19  \w    -48.00 -21.00   0.50    4.35    --  -90.00  45.00-120.00   54
 20  \w    -48.00 -23.00   0.50    4.35    --  -90.00  45.00 -60.00   50
 21  \w    -44.00 -17.00   0.50    4.35    --  -90.00 125.00-180.00   54
 22  \w    -61.00 -20.00   0.50    4.35    --  -90.00  61.00   0.00   82
 23  \w     92.00 176.00   0.50    4.35    --  105.88  15.00  90.00  168
 24  \w     43.00  74.00   0.50    4.35    --  105.88 -61.00-150.00   62
 25  \w     37.00  73.00   0.50    4.35    --  105.88 -61.00 -30.00   72
 26  \w    153.00 178.00   0.50    4.35    --  105.88  30.00 -30.00   50
 27  \w     93.00 134.00   0.50    4.35    --  105.88  30.00 -30.00   82
 28  \w     37.00  70.00   0.50    4.35    --  105.88 -61.00-180.00   66
 29  \w    100.00 148.00   0.50    4.35    --  105.88  15.00-180.00   96
 30  \w     66.00 111.00   0.50    4.35    --  105.88-125.00 -30.00   90
 31  \w     46.00  74.00   0.50    4.35    --  105.88 -61.00 150.00   56
;
_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      -0.0072978000
_diffrn_orient_matrix_UB_12      -0.1798790000
_diffrn_orient_matrix_UB_13      -0.0143404000
_diffrn_orient_matrix_UB_21      -0.0149101000
_diffrn_orient_matrix_UB_22      -0.0180678000
_diffrn_orient_matrix_UB_23      0.0550479000
_diffrn_orient_matrix_UB_31      -0.1813590000
_diffrn_orient_matrix_UB_32      -0.0176531000
_diffrn_orient_matrix_UB_33      -0.0125173000
_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  0.0329
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_Laue_measured_fraction_full 0.892
_diffrn_reflns_Laue_measured_fraction_max 0.820
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            15201
_diffrn_reflns_point_group_measured_fraction_full 0.892
_diffrn_reflns_point_group_measured_fraction_max 0.820
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.792
_diffrn_reflns_theta_min         3.342
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.611
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73877
_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            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.818
_exptl_crystal_description       prism
_exptl_crystal_F_000             1084
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.623
_refine_diff_density_min         -1.116
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     580
_refine_ls_number_reflns         6777
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0539
_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^)+(0.0924P)^2^+4.1008P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1520
_refine_ls_wR_factor_ref         0.1543
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6591
_reflns_number_total             6777
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02777a2.cif
_cod_data_source_block           jp270
_cod_depositor_comments
'Adding full bibliography for 7717638--7717643.cif.'
_cod_database_code               7717640
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C16 H14  N4 Cu Cl2 O8'
_reflns_odcompleteness_completeness 89.42
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.79543
 0.20457
2.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), C18(H18), C19(H19), C20(H20), C21(H21), C24(H24), C25(H25),
  C26(H26), C29(H29), C30(H30), C31(H31), C32(H32)
2.b Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C34(H34A,H34B,H34C)
;
_shelx_res_checksum              95601
_shelx_hkl_checksum              9887
_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 2.090
_oxdiff_exptl_absorpt_empirical_full_min 0.663