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_7700982
_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      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-08-14
_audit_creation_method
;
Olex2 1.2-ac3
(compiled 2017.02.24 svn.r3390 for Rigaku Oxford Diffraction, GUI svn.r5318)
;
_audit_update_record
;
2019-08-14 deposited with the CCDC.    2019-08-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8109(4)
_cell_length_b                   18.5996(6)
_cell_length_c                   8.9913(3)
_cell_measurement_reflns_used    8069
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.1880
_cell_measurement_theta_min      3.5140
_cell_volume                     2142.43(12)
_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      293(2)
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.945
_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  -7.00   0.50   25.00    --   -9.79 -86.00  13.00   52
  2  \w    -32.00  -3.00   0.50   25.00    --   -9.79  86.00 131.00   58
  3  \w     -7.00  34.00   0.50   25.00    --   10.07  86.00 131.00   82
  4  \w    -22.00   3.00   0.50   25.00    --   10.07 -86.00  13.00   50
  5  \w    -67.00   8.00   0.50   25.00    --   -9.79 -57.00   0.00  150
  6  \w    -76.00   2.00   0.50   25.00    --   -9.79 -19.00 -30.00  156
  7  \w    -22.00  51.00   0.50   25.00    --   -9.79  57.00 -30.00  146
  8  \w      0.00  74.00   0.50   25.00    --   10.07  19.00-180.00  148
  9  \w     11.00  57.00   0.50   25.00    --   10.07-125.00 -90.00   92
 10  \w     -9.00  -4.00   0.50   25.00    --   10.07 -99.00 -60.00   10
;
_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  0.0879
_diffrn_reflns_av_unetI/netI     0.0544
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            18328
_diffrn_reflns_point_group_measured_fraction_full 0.824
_diffrn_reflns_point_group_measured_fraction_max 0.754
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.437
_diffrn_reflns_theta_min         3.180
_exptl_absorpt_coefficient_mu    0.881
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52665
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_description       block
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.412
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details
;
 Flack x determined using 784 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.05(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     390
_refine_ls_number_reflns         3701
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0707
_refine_ls_R_factor_gt           0.0487
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0698P)^2^+0.4238P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1260
_refine_ls_wR_factor_ref         0.1429
_reflns_Friedel_coverage         0.500
_reflns_Friedel_fraction_full    0.626
_reflns_Friedel_fraction_max     0.537
_reflns_number_gt                2648
_reflns_number_total             3701
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02834j2.cif
_cod_data_source_block           sub-pan-4-bf42
_cod_depositor_comments
'Adding full bibliography for 7700982--7700985.cif.'
_cod_database_code               7700982
_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. Restrained angles
 F8A-N2-F8
 fixed at 108 with sigma of 0.02
3. Rigid body (RIGU) restrains
 F3, F4, F5A, N1, F5A, N1, N2, N2, N3, N3, N4, N4, F5A, F6, F5A, F5A, F3, B1,
 F4, B1, F7, F8A, F7A, F8A, F7A, B2, F7A, F7A, F4, F7A, F7A, F7A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N1, N1, N2, N2, N3, N3, N4, N4, F3A, B1, F4A, B1, F8, F8A, F8, F8, F3A, F4A,
 F8, F8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: F3(0.5) F3A(0.5) F4(0.5) F4A(0.5) F7(0.5) F7A(0.5) F8(0.5)
 F8A(0.5) F5(0.5) F5A(0.5) C2(0.5) H2A(0.5) H2B(0.5) C3(0.5) H3A(0.5) H3B(0.5)
 C2A(0.5) H2AA(0.5) H2AB(0.5) C3A(0.5) H3AA(0.5) H3AB(0.5) C6(0.5) H6A(0.5)
 H6B(0.5) C5(0.5) H5A(0.5) H5B(0.5) C5A(0.5) H5AA(0.5) H5AB(0.5) C6A(0.5)
 H6AA(0.5) H6AB(0.5) C8(0.5) H8A(0.5) H8B(0.5) C9(0.5) H9A(0.5) H9B(0.5)
 C8A(0.5) H8AA(0.5) H8AB(0.5) C9A(0.5) H9AA(0.5) H9AB(0.5) C11(0.5) H11A(0.5)
 H11B(0.5) C12(0.5) H12A(0.5) H12B(0.5) C11A(0.5) H11C(0.5) H11D(0.5) C12A(0.5)
 H12C(0.5) H12D(0.5) O9(0.2) O9A(0.8)
5.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C2A(H2AA,H2AB), C3A(H3AA,H3AB), C6(H6A,H6B), C5(H5A,
 H5B), C5A(H5AA,H5AB), C6A(H6AA,H6AB), C8(H8A,H8B), C9(H9A,H9B), C8A(H8AA,H8AB),
  C9A(H9AA,H9AB), C11(H11A,H11B), C12(H12A,H12B), C11A(H11C,H11D), C12A(H12C,
 H12D)
5.b Me refined with riding coordinates:
 C7(H7A,H7B,H7C), C4(H4A,H4B,H4C)
5.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C1(H1A,H1B,H1C)
;
_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
;