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_7717641
_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 N5 O4'
_chemical_formula_sum            'C15 H11 Cu N5 O4'
_chemical_formula_weight         388.83
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2yc'
_space_group_name_H-M_alt        'I 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-11-01
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-11-04 deposited with the CCDC.	2024-12-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.053(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3459(7)
_cell_length_b                   9.4549(4)
_cell_length_c                   11.8624(6)
_cell_measurement_reflns_used    3009
_cell_measurement_temperature    100.01(12)
_cell_measurement_theta_max      76.0180
_cell_measurement_theta_min      5.6830
_cell_volume                     1478.20(13)
_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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(12)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.910
_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     33.00  74.00   0.50    0.90    --  105.91 -61.00 -60.00   82
  2  \w     33.00  74.00   0.50    0.90    --  105.91 -61.00 -90.00   82
  3  \w     63.00  91.00   0.50    0.30    --   47.03  19.00 156.00   56
  4  \w    -23.00   2.00   0.50    0.30    --   47.03 -19.00 -10.00   50
  5  \w     48.00  73.00   0.50    0.90    --  105.91 -61.00  60.00   50
  6  \w     93.00 153.00   0.50    0.90    --  105.91  19.00 156.00  120
  7  \w    -51.00 -23.00   0.50    0.90    --  -91.75  61.00 120.00   56
  8  \w    -67.00 -27.00   0.50    0.90    --  -91.75  61.00  90.00   80
  9  \w    -48.00 -23.00   0.50    0.90    --  -91.75  45.00  90.00   50
 10  \w    -46.00 -20.00   0.50    0.90    --  -91.75  45.00 150.00   52
 11  \w    -51.00 -19.00   0.50    0.90    --  -91.75  61.00   0.00   64
 12  \w    -45.00 -20.00   0.50    0.90    --  -91.75  45.00  30.00   50
 13  \w    -48.00 -23.00   0.50    0.90    --  -91.75  45.00 120.00   50
 14  \w    -60.00 -26.00   0.50    0.90    --  -91.75  61.00 -60.00   68
 15  \w    -48.00 -23.00   0.50    0.90    --  -91.75  45.00 -90.00   50
 16  \w    -54.00 -28.00   0.50    0.90    --  -91.75  61.00-120.00   52
 17  \w   -103.00 -45.00   0.50    0.30    --  -47.03 -19.00 -10.00  116
 18  \w   -117.00 -80.00   0.50    0.90    --  -91.75 -19.00 -10.00   74
 19  \w     33.00  94.00   0.50    0.90    --  105.91 -94.00-150.00  122
 20  \w     48.00 103.00   0.50    0.90    --  105.91 -94.00-120.00  110
 21  \w    -23.00  27.00   0.50    0.30    --  -47.03  19.00 156.00  100
 22  \w    -19.00  16.00   0.50    0.30    --  -47.03  19.00 -60.00   70
 23  \w    -40.00   8.00   0.50    0.30    --  -47.03  38.00-150.00   96
;
_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      0.1137509000
_diffrn_orient_matrix_UB_12      -0.0110675000
_diffrn_orient_matrix_UB_13      -0.0086873000
_diffrn_orient_matrix_UB_21      -0.0271061000
_diffrn_orient_matrix_UB_22      -0.0380680000
_diffrn_orient_matrix_UB_23      -0.1273283000
_diffrn_orient_matrix_UB_31      0.0014507000
_diffrn_orient_matrix_UB_32      0.1580387000
_diffrn_orient_matrix_UB_33      -0.0314522000
_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  0.0355
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.910
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3833
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.910
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.409
_diffrn_reflns_theta_min         5.759
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.410
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56760
_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    1.747
_exptl_crystal_description       prism
_exptl_crystal_F_000             788
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.740
_refine_diff_density_min         -0.558
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     143
_refine_ls_number_reflns         1414
_refine_ls_number_restraints     68
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0492
_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/[\s^2^(Fo^2^)+(0.0903P)^2^+2.8494P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1297
_refine_ls_wR_factor_ref         0.1320
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1334
_reflns_number_total             1414
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02777a2.cif
_cod_data_source_block           jp278
_cod_depositor_comments
'Adding full bibliography for 7717638--7717643.cif.'
_cod_database_code               7717641
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Cu O4 N5 H12 C15'
_reflns_odcompleteness_completeness 99.22
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 N3A-O2A
 1.25 with sigma of 0.02
 O1A-N3A
 1.25 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O1 \\sim O1A \\sim N3 \\sim N3A \\sim O2A \\sim O2: within 1.7A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 1.7A
4. Others
 Sof(N3A)=Sof(O1A)=Sof(O2A)=1-FVAR(1)
 Sof(O1)=Sof(O2)=Sof(N3)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C7(H7), C1(H1), C2(H2), C8(H8)
;
_shelx_res_checksum              28950
_shelx_hkl_checksum              53080
_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 1.697
_oxdiff_exptl_absorpt_empirical_full_min 0.536