Catalytic fate of structurally characterized manganese(iii)–salen complexes towards efficient transformation of primary amides to amines or nitriles using hydrosilane
Bandopadhyay, Nilaj; Paramanik, Krishnendu; Sarkar, Gayetri; Chatterjee, Souvik; Roy, Suvojit; Panda, Subhra Jyoti; Purohit, Chandra Shekhar; Biswas, Bhaskar; Das, Hari Sankar; New Journal of Chemistry 47 (2023) 9414–9420; doi:10.1039/D3NJ01183F

data_7062422
_publ_section_title
;
 Catalytic fate of structurally characterized manganese(iii)--salen
 complexes towards efficient transformation of primary amides to amines or
 nitriles using hydrosilane
;
_journal_issue                   19
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              9414
_journal_page_last               9420
_journal_paper_doi               10.1039/D3NJ01183F
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C16 H16 Mn N2 O3, Cl O4, H2 O'
_chemical_formula_sum            'C16 H18 Cl Mn N2 O8'
_chemical_formula_weight         456.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-12-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-02-17 deposited with the CCDC.	2023-04-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.88(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.2081(14)
_cell_length_b                   13.4249(19)
_cell_length_c                   19.416(5)
_cell_measurement_reflns_used    2171
_cell_measurement_temperature    298.0(2)
_cell_measurement_theta_max      32.1410
_cell_measurement_theta_min      2.6410
_cell_volume                     1872.0(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.7f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.7f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.7f (Rigaku OD, 2015)'
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      298.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -69.00 118.20   0.30   30.00    --   29.89  54.00 120.00  624
  2  \w    -69.00 118.20   0.30   30.00    --   29.89  54.00-150.00  624
  3  \w    -69.00 118.20   0.30   30.00    --   29.89  54.00 120.00  624
  4  \w    -69.00  66.00   0.30   30.00    --   29.89  54.00 -30.00  450
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini (ROW)'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0169878000
_diffrn_orient_matrix_UB_12      0.0028071000
_diffrn_orient_matrix_UB_13      0.0354157000
_diffrn_orient_matrix_UB_21      0.0971179000
_diffrn_orient_matrix_UB_22      -0.0024728000
_diffrn_orient_matrix_UB_23      0.0093662000
_diffrn_orient_matrix_UB_31      0.0055296000
_diffrn_orient_matrix_UB_32      0.0527045000
_diffrn_orient_matrix_UB_33      -0.0014514000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1344
_diffrn_reflns_av_unetI/netI     0.0692
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            20292
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         2.595
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.896
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear reddish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_description       block
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.932
_refine_diff_density_min         -0.444
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         3284
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.1166
_refine_ls_R_factor_gt           0.0883
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1665P)^2^+0.9184P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2304
_refine_ls_wR_factor_ref         0.2708
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2264
_reflns_number_total             3284
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj01183f2.cif
_cod_data_source_block           nb_4_rt
_cod_depositor_comments
'Adding full bibliography for 7062422--7062423.cif.'
_cod_original_cell_volume        1872.0(6)
_cod_database_code               7062422
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_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 O(H,H) groups
2.a Free rotating group:
 O009(H00Q,H00R)
2.b Rotating group:
 O005(H00A,H00B)
2.c Secondary CH2 refined with riding coordinates:
 C00J(H00C,H00J), C00M(H00M,H00N)
2.d Aromatic/amide H refined with riding coordinates:
 C00D(H00D), C00E(H00E), C00F(H00F), C00G(H00G), C00H(H00H), C00I(H00I),
 C00K(H00K), C00L(H00L), C00N(H00O), C00O(H00P)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
;
_oxdiff_exptl_absorpt_empirical_full_max 1.390
_oxdiff_exptl_absorpt_empirical_full_min 0.729