Designing a NNO-manganese complex overcoming steric constraints in (de)hydrogenative coupling.
Mondal, Avijit; Phukan, Hirak Jyoti; Mohar, Kailash; Pal, Debjyoti; Sharma, Rahul; Purkayastha, Siddhartha; Guha, Ankur Kanti; Srimani, Dipankar; Chemical communications (Cambridge, England) 61 (2025) 4796–4799; doi:10.1039/d5cc00048c

data_7134288
_publ_section_title
;
 Designing a NNO-manganese complex overcoming steric constraints in
 (de)hydrogenative coupling.
;
_journal_issue                   25
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4796
_journal_page_last               4799
_journal_paper_doi               10.1039/d5cc00048c
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'Br, C12 H14 Mn N2 O4'
_chemical_formula_sum            'C12 H14 Br Mn N2 O4'
_chemical_formula_weight         385.10
_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   mixed
_audit_creation_date             2023-09-06
_audit_creation_method
;
Olex2 1.5
(compiled 2021.07.19 svn.r715e62df for OlexSys, GUI svn.r6380)
;
_audit_update_record
;
2024-02-06 deposited with the CCDC.	2025-02-25 downloaded from the CCDC.
;
_cell_angle_alpha                79.837(3)
_cell_angle_beta                 75.722(2)
_cell_angle_gamma                71.616(4)
_cell_formula_units_Z            2
_cell_length_a                   7.3733(5)
_cell_length_b                   8.8785(8)
_cell_length_c                   12.8155(14)
_cell_measurement_reflns_used    3242
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.29
_cell_measurement_theta_min      2.43
_cell_volume                     767.09(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.940
_diffrn_measured_fraction_theta_max 0.940
_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  0.0520
_diffrn_reflns_av_unetI/netI     0.0578
_diffrn_reflns_Laue_measured_fraction_full 0.940
_diffrn_reflns_Laue_measured_fraction_max 0.940
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6915
_diffrn_reflns_point_group_measured_fraction_full 0.940
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_theta_full        24.992
_diffrn_reflns_theta_max         24.992
_diffrn_reflns_theta_min         2.431
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.477
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.667
_exptl_crystal_description       block
_exptl_crystal_F_000             384
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.451
_refine_diff_density_min         -0.557
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         2542
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0413
_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^)+(0.0585P)^2^+0.1287P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1070
_refine_ls_wR_factor_ref         0.1130
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2123
_reflns_number_total             2542
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc00048c2.cif
_cod_data_source_block           amds350nme_ds_0m_a
_cod_depositor_comments
'Adding full bibliography for 7134286--7134288.cif.'
_cod_database_code               7134288
_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. Restrained distances
 H003-O003
 0.87 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C009(H00A,H00B), C00B(H00C,H00D), C00C(H00E,H00F)
3.b Aromatic/amide H refined with riding coordinates:
 C008(H008), C00E(H00G), C00G(H00H), C00H(H00I)
3.c Idealised Me refined as rotating group:
 C00I(H00J,H00K,H00L)
;
_shelx_res_checksum              18266
_shelx_hkl_checksum              97568
_olex2_submission_special_instructions 'No special instructions were received'