Nitric oxide monooxygenation (NOM) reaction of cobalt-nitrosyl {Co(NO)}8 to CoII-nitrito {CoII(NO2−)}: base induced hydrogen gas (H2) evolution
Das, Sandip; Kulbir,; Ghosh, Somnath; Chandra Sahoo, Subash; Kumar, Pankaj; Chemical Science 11 (2020) 5037–5042; doi:10.1039/D0SC01572E

data_1557898
_publ_section_title
;
 Nitric oxide monooxygenation (NOM) reaction of cobalt-nitrosyl {Co(NO)}8
 to CoII-nitrito {CoII(NO2&#x2212;)}: base induced hydrogen gas (H2)
 evolution
;
_journal_issue                   19
_journal_name_full               'Chemical Science'
_journal_page_first              5037
_journal_page_last               5042
_journal_paper_doi               10.1039/D0SC01572E
_journal_volume                  11
_journal_year                    2020
_chemical_compound_source        synthesized
_chemical_formula_moiety         'C12 H28 Co N5 O2, B F4'
_chemical_formula_sum            'C12 H28 B Co F4 N5 O2'
_chemical_formula_weight         420.13
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-12-28
_audit_creation_method
;
Olex2 1.2-ac3
(compiled 2017.02.24 svn.r3390 for Rigaku Oxford Diffraction, GUI svn.r5318)
;
_audit_update_record
;
2019-12-28 deposited with the CCDC.	2020-04-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.0883(2)
_cell_length_b                   14.8329(3)
_cell_length_c                   19.5325(3)
_cell_measurement_reflns_used    30109
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.3180
_cell_measurement_theta_min      3.3190
_cell_volume                     3791.99(11)
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.977
_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      7.00  56.00   0.50   15.00    --   -9.95  30.00 154.00   98
  2  \w    -48.00 -20.00   0.50   15.00    --   -9.95 -30.00  -5.00   56
  3  \w    -56.00 -11.00   0.50   15.00    --   10.22 -30.00  -5.00   90
  4  \w     35.00  61.00   0.50   15.00    --   10.22  30.00 154.00   52
  5  \w    -56.00 -19.00   0.50   15.00    --   -9.95 125.00 120.00   74
  6  \w    -58.00 -23.00   0.50   15.00    --   -9.95 125.00 -90.00   70
  7  \w    -73.00 -27.00   0.50   15.00    --   -9.95 -57.00  60.00   92
  8  \w    -47.00 -22.00   0.50   15.00    --   -9.95 125.00   0.00   50
  9  \w    -49.00   7.00   0.50   15.00    --   -9.95 -57.00 -30.00  112
 10  \w    -49.00 -23.00   0.50   15.00    --   -9.95 125.00-120.00   52
 11  \w    -30.00   1.00   0.50   15.00    --   10.22 121.00 147.94   62
 12  \w    -33.00   0.00   0.50   15.00    --   10.22 118.00-135.82   66
 13  \w     49.00  74.00   0.50   15.00    --   10.22  38.00 -60.00   50
 14  \w    -37.00  -5.00   0.50   15.00    --   10.22 124.00 -37.75   64
 15  \w    -60.00  22.00   0.50   15.00    --   10.22 -19.00-150.00  164
 16  \w      5.00  36.00   0.50   15.00    --   10.22  38.00 -60.00   62
 17  \w     -2.00  77.00   0.50   15.00    --   10.22  19.00  30.00  158
 18  \w     -5.00  56.00   0.50   15.00    --   10.22  57.00 150.00  122
 19  \w     -9.00  40.00   0.50   15.00    --   10.22 -99.00-150.00   98
 20  \w    -32.00  -2.00   0.50   15.00    --   10.22 116.00  71.85   60
 21  \w      8.00  43.00   0.50   15.00    --   10.22 -99.00 -90.00   70
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0196854000
_diffrn_orient_matrix_UB_12      0.0442373000
_diffrn_orient_matrix_UB_13      0.0038917000
_diffrn_orient_matrix_UB_21      0.0459669000
_diffrn_orient_matrix_UB_22      -0.0179698000
_diffrn_orient_matrix_UB_23      0.0135951000
_diffrn_orient_matrix_UB_31      0.0209650000
_diffrn_orient_matrix_UB_32      -0.0021481000
_diffrn_orient_matrix_UB_33      -0.0334459000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_av_unetI/netI     0.0168
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            57112
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.390
_diffrn_reflns_theta_min         3.325
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.958
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70839
_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            red
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_description       block
_exptl_crystal_F_000             1752
_exptl_crystal_recrystallization_method 'slow evaporation'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.698
_refine_diff_density_min         -0.397
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         4208
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.177
_refine_ls_R_factor_all          0.0792
_refine_ls_R_factor_gt           0.0623
_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^)+(0.0964P)^2^+3.7491P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1908
_refine_ls_wR_factor_ref         0.2051
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3007
_reflns_number_total             4208
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc01572e2.cif
_cod_data_source_block           Co-BF4
_cod_depositor_comments
;Adding full bibliography for 1557898.cif.

 Adding full bibliography for 1557898.cif.
;
_cod_database_code               1557898
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Co B F C H N O'
_diffrn_oxdiff_ac3_digest_frames
;
0197eeb08c3a60edf726793378415987da000253582
;
_diffrn_oxdiff_ac3_digest_hkl
;
01a427163ced6726a2332d16e91ade0b193575
;
_reflns_odcompleteness_completeness 99.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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. Rigid body (RIGU) restrains
 C2, C3, C5, C6, C8, C9, C11, C12, N3, C6, N3, C8, N2, C3, N2, C5, N4, C9, N4,
 C11, N1, C2, N1, C12, C6, C5, C6, C9, C8, C3, C2, C5, C12, C11, C11, C12, C2,
 C3, C9, C11, C2, C9, C11, C11, C8, C9, C5, C6
 with sigma for 1-2 distances of 0.00005 and sigma for 1-3 distances of 0.00005
 C2A, C3A, C5A, C6A, C8A, C9A, C11A, C12A, N3, C6A, N3, C8A, N2, C3A, N2, C5A,
 N4, C9A, N4, C11A, N1, C2A, N1, C12A, C6A, C5A, C9A, C8A, C3A, C2A, C5A, C12A,
 C11A, C11A, C12A, C2A, C3A, C12A, C8A, C9A, C11A, C9A, C11A, C9A, C11A, C8A,
 C5A, C6A
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
3. Others
 Fixed Sof: C2(0.6) H2A(0.6) H2B(0.6) C2A(0.4) H2AA(0.4) H2AB(0.4) C3(0.6)
 H3A(0.6) H3B(0.6) C3A(0.4) H3AA(0.4) H3AB(0.4) C5(0.6) H5A(0.6) H5B(0.6)
 C5A(0.4) H5AA(0.4) H5AB(0.4) C6(0.6) H6A(0.6) H6B(0.6) C6A(0.4) H6AA(0.4)
 H6AB(0.4) C8(0.6) H8A(0.6) H8B(0.6) C8A(0.4) H8AA(0.4) H8AB(0.4) C9(0.6)
 H9A(0.6) H9B(0.6) C9A(0.4) H9AA(0.4) H9AB(0.4) C11(0.6) H11A(0.6) H11B(0.6)
 C11A(0.4) H11C(0.4) H11D(0.4) C12(0.6) H12A(0.6) H12B(0.6) C12A(0.4) H12C(0.4)
 H12D(0.4)
4.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C2A(H2AA,H2AB), C3(H3A,H3B), C3A(H3AA,H3AB), C5(H5A,H5B),
 C5A(H5AA,H5AB), C6(H6A,H6B), C6A(H6AA,H6AB), C8(H8A,H8B), C8A(H8AA,H8AB),
 C9(H9A,H9B), C9A(H9AA,H9AB), C11(H11A,H11B), C11A(H11C,H11D), C12(H12A,H12B),
 C12A(H12C,H12D)
4.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C1(H1A,H1B,H1C), C7(H7A,H7B,H7C), C4(H4A,H4B,H4C)
;
_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 1.448
_oxdiff_exptl_absorpt_empirical_full_min 0.774