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_7717642
_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 H16 Cu N3 O3, F6 P'
_chemical_formula_sum            'C17 H16 Cu F6 N3 O3 P'
_chemical_formula_weight         518.84
_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'
_atom_sites_solution_hydrogens   mixed
_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                90
_cell_angle_beta                 101.129(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1663(2)
_cell_length_b                   26.6284(4)
_cell_length_c                   7.25480(10)
_cell_measurement_reflns_used    6184
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.7190
_cell_measurement_theta_min      3.2850
_cell_volume                     1927.03(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_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      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.935
_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    -74.00 -25.00   0.50    5.10    --  -47.28  88.00 -97.00   98
  2  \w      0.00  46.00   0.50    5.10    --   47.28 -88.00 146.00   92
  3  \w   -157.00 -98.00   0.50   19.09    --  -91.75 -88.00 146.00  118
  4  \w    -71.00 -45.00   0.50   19.09    --  -91.75  88.00 -97.00   52
  5  \w     34.00  73.00   0.50   19.09    --  105.91 -88.00 146.00   78
  6  \w    121.00 147.00   0.50   19.09    --  105.91  88.00 -97.00   52
  7  \w    -22.00  28.00   0.50    5.10    --  -47.28  19.00 -30.00  100
  8  \w    -21.00  23.00   0.50    5.10    --  -47.28  19.00  30.00   88
  9  \w   -118.00 -78.00   0.50    5.10    --  -47.28-125.00-150.00   80
 10  \w   -114.00 -76.00   0.50    5.10    --  -47.28-125.00 -60.00   76
 11  \w    -46.00 -21.00   0.50   19.09    --  -91.75  45.00-180.00   50
 12  \w    -48.00 -23.00   0.50   19.09    --  -91.75  45.00  60.00   50
 13  \w    -67.00 -27.00   0.50   19.09    --  -91.75  61.00-120.00   80
 14  \w    -85.00 -28.00   0.50   19.09    --  -91.75 125.00 150.00  114
 15  \w    -47.00 -20.00   0.50   19.09    --  -91.75  45.00 120.00   54
 16  \w     33.00 107.00   0.50   19.09    --  105.91 -77.00 -60.00  148
 17  \w     33.00  58.00   0.50   19.09    --  105.91 -61.00 -30.00   50
 18  \w     35.00  70.00   0.50   19.09    --  105.91 -61.00-150.00   70
 19  \w     34.00  59.00   0.50   19.09    --  105.91 -61.00  30.00   50
 20  \w     82.00 106.50   0.50   19.09    --  105.91-125.00 120.00   49
 21  \w     41.00  66.00   0.50   19.09    --  105.91-125.00 120.00   50
 22  \w     38.00 103.00   0.50   19.09    --  105.91 -77.00  30.00  130
 23  \w     34.00  63.00   0.50   19.09    --  105.91 -61.00 -60.00   58
 24  \w     81.00  94.00   0.50   19.09    --  105.91 -88.00 146.00   26
;
_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      -0.0817276000
_diffrn_orient_matrix_UB_12      -0.0474367000
_diffrn_orient_matrix_UB_13      -0.0683957000
_diffrn_orient_matrix_UB_21      0.1208630000
_diffrn_orient_matrix_UB_22      -0.0215836000
_diffrn_orient_matrix_UB_23      -0.0732080000
_diffrn_orient_matrix_UB_31      0.0505137000
_diffrn_orient_matrix_UB_32      -0.0251410000
_diffrn_orient_matrix_UB_33      0.1918373000
_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  0.0301
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.935
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            12215
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.935
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.501
_diffrn_reflns_theta_min         3.319
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.177
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_correction_T_min  0.924
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.788
_exptl_crystal_description       prism
_exptl_crystal_F_000             1044
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.080
_refine_diff_density_min         -0.447
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         3782
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0433
_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^)+(0.0674P)^2^+2.0832P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1154
_refine_ls_wR_factor_ref         0.1196
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3342
_reflns_number_total             3782
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02777a2.cif
_cod_data_source_block           jppostcpcacoh
_cod_depositor_comments
'Adding full bibliography for 7717638--7717643.cif.'
_cod_database_code               7717642
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C17 N3 Cu Cl O7 H15'
_shelx_estimated_absorpt_t_max   0.857
_shelx_estimated_absorpt_t_min   0.683
_reflns_odcompleteness_completeness 99.43
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Restrained distances
 H1B-H1A
 1.54 with sigma of 0.02
 H1A-O1
 0.95 with sigma of 0.02
 H1B-O1
 0.95 with sigma of 0.02
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)
2.b Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C)
;
_shelx_res_checksum              35247
_shelx_hkl_checksum              14663
_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 1.449
_oxdiff_exptl_absorpt_empirical_full_min 0.810