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_7712603
_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         'C19 H29 Cl0.18 Mn N5.82 O3, C24 H20 B'
_chemical_formula_sum            'C43 H49 B Cl0.18 Mn N5.82 O3'
_chemical_formula_weight         767.49
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-02-27
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-02-27 deposited with the CCDC.	2023-03-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.045(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.5034(10)
_cell_length_b                   11.0969(7)
_cell_length_c                   22.2792(13)
_cell_measurement_reflns_used    9136
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      28.25
_cell_measurement_theta_min      2.57
_cell_volume                     3921.2(4)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0454
_diffrn_reflns_av_unetI/netI     0.0193
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            131461
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.306
_diffrn_reflns_theta_min         2.240
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.396
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.7114
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0913 before and 0.0526 after correction.
The Ratio of minimum to maximum transmission is 0.9540.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_description       block
_exptl_crystal_F_000             1619
_refine_diff_density_max         0.489
_refine_diff_density_min         -0.369
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     536
_refine_ls_number_reflns         9714
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0353
_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^)+(0.0409P)^2^+2.2708P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0885
_refine_ls_wR_factor_ref         0.0915
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8940
_reflns_number_total             9714
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00159h2.cif
_cod_data_source_block           mo_mn_n3_nrte_bp_0m_a
_cod_database_code               7712603
_shelx_shelxl_version_number     2019/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 O4, O4A, N6, O3, Cl6A, O3A, O1, O1A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
O3A \\sim O1A \\sim O1 \\sim O3 \\sim O4A \\sim O4: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
Cl6A: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002
within 2A
Uanis(O4A) \\sim Ueq, Uanis(N6) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(O4) \\sim
Ueq, Uanis(Cl6A) \\sim Ueq, Uanis(O1A) \\sim Ueq, Uanis(O3A) \\sim Ueq,
Uanis(O1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Cl6A) \\sim Ueq, Uanis(O4A) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(Cl6A) \\sim Ueq: with sigma of 0.00001 and sigma for terminal atoms of
0.00002
Uanis(N6) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Others
 Sof(O4A)=1-FVAR(1)
 Sof(O4)=FVAR(1)
 Fixed Sof: O3(0.8) O1(0.74) N6(0.82) Cl6A(0.18) O3A(0.18) O1A(0.18) O2(0.1)
5.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,
 H11B)
5.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C3(H3), C2(H2), C1(H1), C16(H16), C15(H15), C14(H14), C13(H13),
 C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C27(H27), C28(H28), C29(H29),
  C30(H30), C31(H31), C33(H33), C34(H34), C35(H35), C36(H36), C37(H37),
 C39(H39), C40(H40), C41(H41), C42(H42), C43(H43)
5.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              39712
_shelx_fab_checksum              29208
_olex2_submission_special_instructions 'No special instructions were received'