Exploring the Nitric Oxide Dioxygenation (NOD) Reactions of Manganese-peroxo Complexes
Das, Sandip; C S, Akshaya Keerthi; kulbir, Kulbir; Singh, Shivangi; Roy, Soumik; Singh, Raman; Ghosh, Somnath; Kumar, Pankaj; Dalton Transactions  (2023) –; doi:10.1039/D3DT00159H

data_7712602
_publ_section_title
;
 Exploring the Nitric Oxide Dioxygenation (NOD) Reactions of
 Manganese-peroxo Complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00159H
_journal_year                    2023
_chemical_formula_moiety         'C21 H25 Mn N6 O3, C24 H20 B'
_chemical_formula_sum            'C45 H45 B Mn N6 O3'
_chemical_formula_weight         783.64
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-12-27
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-01-18 deposited with the CCDC.	2023-03-08 downloaded from the CCDC.
;
_cell_angle_alpha                89.775(4)
_cell_angle_beta                 84.127(4)
_cell_angle_gamma                67.815(4)
_cell_formula_units_Z            4
_cell_length_a                   11.2760(12)
_cell_length_b                   14.8557(15)
_cell_length_c                   25.600(3)
_cell_measurement_reflns_used    9634
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.149
_cell_measurement_theta_min      2.175
_cell_volume                     3947.2(8)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2016)'
_computing_data_collection       'SAINT V8.40B (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'PHOTON III DUO'
_diffrn_measurement_method       Mo
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            13956
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.104
_diffrn_reflns_theta_max         25.104
_diffrn_reflns_theta_min         0.800
_exptl_absorpt_coefficient_mu    0.384
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6894
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1111 before and 0.0781 after correction.
The Ratio of minimum to maximum transmission is 0.9251.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1644
_exptl_crystal_size_max          0.423
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.298
_refine_diff_density_max         0.688
_refine_diff_density_min         -0.780
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1012
_refine_ls_number_reflns         13956
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0807
_refine_ls_R_factor_gt           0.0732
_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^)+(0.0625P)^2^+21.1360P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2022
_refine_ls_wR_factor_ref         0.2062
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12366
_reflns_number_total             13956
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00159h2.cif
_cod_data_source_block           mo_mn_3p_nrte_3_0m_a
_cod_depositor_comments
;

2025-03-07
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         74.63
_cod_original_formula_moiety         '0.095(C21 H25 Mn N6 O3), 0.095(C24 H20 B)'
_cod_original_formula_units_Z            42
_cod_original_cell_volume        3947.2(7)
_cod_original_formula_sum        'C4.29 H4.29 B0.10 Mn0.10 N0.57 O0.29'
_cod_database_code               7712602
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.78662
 0.21338
2.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C6(H6A,H6B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B),
 C28(H28A,H28B), C27(H27A,H27B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B)
2.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C11(H11), C10(H10), C9(H9), C4(H4), C3(H3), C2(H2), C1(H1),
 C20(H20), C19(H19), C18(H18), C17(H17), C30(H30), C31(H31), C32(H32), C33(H33),
  C22(H22), C23(H23), C24(H24), C25(H25), C38(H38), C39(H39), C40(H40),
 C41(H41), C44(H44), C45(H45), C46(H46), C47(H47), C48(H48), C50(H50), C51(H51),
  C52(H52), C53(H53), C54(H54), C56(H56), C57(H57), C58(H58), C59(H59),
 C60(H60), C62(H62), C63(H63), C64(H64), C65(H65), C66(H66), C68(H68), C69(H69),
  C70(H70), C71(H71), C72(H72), C74(H74), C75(H75), C76(H76), C77(H77),
 C78(H78), C80(H80), C81(H81), C82(H82), C83(H83), C84(H84), C86(H86), C87(H87),
  C88(H88), C89(H89), C90(H90)
2.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C42(H42A,H42B,H42C)
;
_shelx_res_checksum              91203
_olex2_submission_special_instructions 'No special instructions were received'