Finding a new pathway for acid-induced nitrite reduction reaction: formation of nitric oxide with hydrogen peroxide.
Puthiyaveetil Yoosaf, Mohammed Ajmal; Ghosh, Somnath; Narayan, Yatheesh; Yadav, Munendra; Sahoo, Subash Chandra; Kumar, Pankaj; Dalton transactions (Cambridge, England : 2003) 48 (2019) 13916–13920; doi:10.1039/c9dt02834j

data_7700985
_publ_section_title
;
 Finding a new pathway for acid-induced nitrite reduction reaction:
 formation of nitric oxide with hydrogen peroxide.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13916
_journal_page_last               13920
_journal_paper_doi               10.1039/c9dt02834j
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C12 H28 Co N5 O, 2(B F4)'
_chemical_formula_sum            'C12 H28 B2 Co F8 N5 O'
_chemical_formula_weight         490.94
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-08-01
_audit_creation_method
;
Olex2 1.2-ac3
(compiled 2017.02.24 svn.r3390 for Rigaku Oxford Diffraction, GUI svn.r5318)
;
_audit_update_record
;
2019-08-02 deposited with the CCDC.    2019-08-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 89.9861(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.91858(15)
_cell_length_b                   12.5051(2)
_cell_length_c                   18.4063(3)
_cell_measurement_reflns_used    16055
_cell_measurement_temperature    123(4)
_cell_measurement_theta_max      27.3200
_cell_measurement_theta_min      3.4250
_cell_volume                     2052.81(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.953
_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    -26.00  10.00   0.50   10.00    --   -9.95  57.00-150.00   72
  2  \w    -54.00 -11.00   0.50   10.00    --   -9.95 125.00-120.00   86
  3  \w     15.00  42.00   0.50   10.00    --   -9.95  57.00-150.00   54
  4  \w    -57.00  -9.00   0.50   10.00    --   -9.95 125.00  90.00   96
  5  \w    -36.00 -10.00   0.50   10.00    --   -9.95 125.00 -90.00   52
  6  \w    -50.00 -22.00   0.50   10.00    --   -9.95 125.00  30.00   56
  7  \w    -51.00  13.00   0.50   10.00    --   10.22 -57.00  90.00  128
  8  \w     28.00  59.00   0.50   10.00    --   10.22-125.00 -90.00   62
  9  \w    -40.00  -7.00   0.50   10.00    --   10.22 131.00 -98.81   66
 10  \w     -7.00  74.00   0.50   10.00    --   10.22  57.00  60.00  162
 11  \w    -28.00   2.00   0.50   10.00    --   10.22 119.00  72.91   60
 12  \w    -47.00  20.00   0.50   10.00    --   10.22 -38.00-150.00  134
 13  \w    -33.00  81.00   0.50   10.00    --   10.22   0.00  60.00  228
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            22856
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.396
_diffrn_reflns_theta_min         3.258
_exptl_absorpt_coefficient_mu    0.920
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92668
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_description       block
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.530
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         4442
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0370
_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^)+(0.0354P)^2^+1.6993P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0877
_refine_ls_wR_factor_ref         0.0911
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3866
_reflns_number_total             4442
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02834j2.cif
_cod_data_source_block           sub-pan-3-bf42
_cod_depositor_comments
'Adding full bibliography for 7700982--7700985.cif.'
_cod_database_code               7700985
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: F3(0.5) F3A(0.5) F4(0.5) F4A(0.5) C3(0.5) H3A(0.5) H3B(0.5)
 C3A(0.5) H3AA(0.5) H3AB(0.5) C4(0.5) H4A(0.5) H4B(0.5) C4A(0.5) H4AA(0.5)
 H4AB(0.5) C7(0.5) H7A(0.5) H7B(0.5) C7A(0.5) H7AA(0.5) H7AB(0.5) C8(0.5)
 H8A(0.5) H8B(0.5) C8A(0.5) H8AA(0.5) H8AB(0.5) C11(0.5) H11A(0.5) H11B(0.5)
 C11A(0.5) H11C(0.5) H11D(0.5) C12(0.5) H12A(0.5) H12B(0.5) C12A(0.5) H12C(0.5)
 H12D(0.5) C15(0.5) H15A(0.5) H15B(0.5) C15A(0.5) H15C(0.5) H15D(0.5) C16(0.5)
 H16A(0.5) H16B(0.5) C16A(0.5) H16C(0.5) H16D(0.5) F7(0.55) F7A(0.45) F8(0.45)
 F8A(0.55)
3.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C3A(H3AA,H3AB), C4(H4A,H4B), C4A(H4AA,H4AB), C7(H7A,H7B),
 C7A(H7AA,H7AB), C8(H8A,H8B), C8A(H8AA,H8AB), C11(H11A,H11B), C11A(H11C,H11D),
 C12(H12A,H12B), C12A(H12C,H12D), C15(H15A,H15B), C15A(H15C,H15D), C16(H16A,
 H16B), C16A(H16C,H16D)
3.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C14(H14A,H14B,H14C), C2(H2A,H2B,H2C), C6(H6A,H6B,H6C)
;
_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
;