Mechanistic Insights of Nitric Oxide Oxygenation (NOO) Reactions of {CrNO}5 & {CoNO}8
C S, Akshaya Keerthi; Das, Sandip; kulbir, Kulbir; Bhardwaj, Prabhakar; Sk, Md Palashuddin; Kumar, Pankaj; Dalton Transactions  (2023) –; doi:10.1039/D3DT03177B

data_7714242
_publ_section_title
;
 Mechanistic Insights of Nitric Oxide Oxygenation (NOO) Reactions of
 {CrNO}5 &amp; {CoNO}8
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT03177B
_journal_year                    2023
_chemical_formula_moiety         'C20 H28 Co N6, 2(C24 H20 B)'
_chemical_formula_sum            'C68 H68 B2 Co N6'
_chemical_formula_weight         1049.83
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-09-08
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-09-10 deposited with the CCDC.	2023-10-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 133.598(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.9696(16)
_cell_length_b                   37.384(3)
_cell_length_c                   18.0414(11)
_cell_measurement_reflns_used    9998
_cell_measurement_temperature    297.0
_cell_measurement_theta_max      21.62
_cell_measurement_theta_min      2.25
_cell_volume                     12196.2(15)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_diffrn_ambient_temperature      297.0
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_av_unetI/netI     0.0468
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            36861
_diffrn_reflns_point_group_measured_fraction_full 0.943
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_theta_full        24.430
_diffrn_reflns_theta_max         24.430
_diffrn_reflns_theta_min         1.985
_diffrn_source                   Mo
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.326
_exptl_absorpt_correction_T_max  0.7447
_exptl_absorpt_correction_T_min  0.7065
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0857 before and 0.0616 after correction.
The Ratio of minimum to maximum transmission is 0.9487.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.144
_exptl_crystal_description       Plate
_exptl_crystal_F_000             4440
_refine_diff_density_max         0.358
_refine_diff_density_min         -0.194
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.19(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1396
_refine_ls_number_reflns         13980
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0486
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0926P)^2^+1.2552P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1328
_refine_ls_wR_factor_ref         0.1424
_reflns_Friedel_coverage         0.890
_reflns_Friedel_fraction_full    0.889
_reflns_Friedel_fraction_max     0.889
_reflns_number_gt                11688
_reflns_number_total             13980
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03177b2.cif
_cod_data_source_block           mo_co_2py_no3_0ma_a
_cod_original_cell_volume        12196.1(15)
_cod_database_code               7714242
_shelx_shelxl_version_number     2019/1
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.81111
 0.18889
2. Uiso/Uaniso restraints and constraints
Uanis(Co1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C44) \\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(C66) \\sim Ueq, Uanis(N9)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3.a Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C43(H43A,H43B), C48(H48A,H48B), C49(H49A,H49B), C50(H50A,
 H50B), C65(H65A,H65B), C66(H66A,H66B), C76(H76A,H76B)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C6(H6), C7(H7), C8(H8), C10(H10), C12(H12),
 C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C21(H21),
  C22(H22), C23(H23), C24(H24), C26(H26), C27(H27), C29(H29), C30(H30),
 C31(H31), C32(H32), C33(H33), C34(H34), C35(H35), C39(H39), C40(H40), C41(H41),
  C42(H42), C44(H44), C51(H51), C53(H53), C54(H54), C55(H55), C56(H56),
 C62(H62), C63(H63), C64(H64), C69(H69), C70(H70), C71(H71), C72(H72), C79(H79),
  C80(H80), C81(H81), C83(H83), C84(H84), C85(H85), C86(H86), C87(H87),
 C88(H88), C89(H89), C90(H90), C91(H91), C93(H93), C94(H94), C95(H95), C96(H96),
  C97(H97), C99(H99), C100(H100), C101(H101), C102(H102), C103(H103),
 C105(H105), C106(H106), C107(H107), C108(H108), C109(H109), C111(H111),
 C112(H112), C113(H113), C114(H114), C115(H115), C116(H116), C117(H117),
 C119(H119), C120(H120), C121(H121), C122(H122), C124(H124), C125(H125),
 C127(H127), C128(H128), C129(H129), C130(H130), C131(H131), C132(H132),
 C133(H133), C134(H134), C135(H135), C136(H136)
3.c Idealised Me refined as rotating group:
 C45(H45A,H45B,H45C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C61(H61A,H61B,
 H61C), C68(H68A,H68B,H68C), C74(H74A,H74B,H74C), C75(H75A,H75B,H75C), C77(H77A,
 H77B,H77C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              31291
_shelx_fab_checksum              36213
_olex2_submission_special_instructions 'No special instructions were received'