Redox-active Ligand Based Mn(I)-Catalyst for Hydrosilylative Ester Reduction
Mandal, Swadhin K.; Chakraborty, Soumi; Das, Arpan; Chemical Communications  (2021) –; doi:10.1039/D1CC05614J

data_7129190
_publ_section_title
;
 Redox-active Ligand Based Mn(I)-Catalyst for Hydrosilylative Ester
 Reduction
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC05614J
_journal_year                    2021
_chemical_formula_moiety         'B F4, C22 H14 Mn N2 O4'
_chemical_formula_sum            'C22 H14 B F4 Mn N2 O4'
_chemical_formula_weight         512.10
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-07-16
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-08-05 deposited with the CCDC.	2021-11-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.311(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7249(7)
_cell_length_b                   14.4773(7)
_cell_length_c                   13.6836(6)
_cell_measurement_reflns_used    7163
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      65.9650
_cell_measurement_theta_min      4.1810
_cell_volume                     2075.8(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9580
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_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    -14.00 100.00   1.00    1.00    --   24.33  57.00-180.00  114
  2  \w     55.00 119.00   1.00    1.00    --   24.33-178.00 150.00   64
  3  \w     57.00 119.00   1.00    1.00    --   24.33 178.00 -60.00   62
  4  \w    -14.00 100.00   1.00    1.00    --   24.33  57.00 -60.00  114
  5  \w     79.00 149.00   1.00    3.00    --   66.17 151.00 -85.00   70
  6  \w    -10.00 103.00   1.00    3.00    --   66.17 -61.00-120.00  113
  7  \w    -13.00 114.00   1.00    3.00    --   66.17 -45.00-150.00  127
  8  \w    100.00 152.00   1.00    3.00    --   66.17 111.00 -30.00   52
  9  \w     57.00 150.00   1.00    3.00    --   66.17 178.00-180.00   93
 10  \w     19.00 146.00   1.00    3.00    --   66.17  45.00 -60.00  127
 11  \w     65.00 178.00   1.00    3.00    --  108.00  77.00 -60.00  113
 12  \w     23.00 151.00   1.00    3.00    --  108.00 -77.00-180.00  128
 13  \w     86.00 178.00   1.00    3.00    --  108.00 138.00  60.00   92
 14  \w     71.00 178.00   1.00    3.00    --  108.00  65.00 -30.00  107
 15  \w     21.00 113.00   1.00    3.00    --  108.00-104.00  90.00   92
 16  \w    101.00 178.00   1.00    3.00    --  108.00 104.00-180.00   77
 17  \w     58.00 178.00   1.00    3.00    --  108.00  43.00 -90.00  120
 18  \w    101.00 178.00   1.00    3.00    --  108.00 104.00 120.00   77
 19  \w     71.00 178.00   1.00    3.00    --  108.00  65.00-120.00  107
 20  \w     21.00 113.00   1.00    3.00    --  108.00-104.00-180.00   92
 21  \w     26.00 120.00   1.00    3.00    --  108.00-122.00  31.00   94
 22  \w     23.00 151.00   1.00    3.00    --  108.00 -77.00  30.00  128
 23  \w     86.00 178.00   1.00    3.00    --  108.00 138.00  90.00   92
 24  \w     86.00 178.00   1.00    3.00    --  108.00 138.00 150.00   92
 25  \w     31.00 147.00   1.00    3.00    --  108.00 -54.00 150.00  116
 26  \w    -57.00  80.00   1.00    1.00    --   24.33 -38.00-150.00  137
 27  \w    -14.00 100.00   1.00    1.00    --   24.33  57.00  60.00  114
 28  \w    -52.00  62.00   1.00    1.00    --   24.33 -57.00  60.00  114
 29  \w     19.00 146.00   1.00    3.00    --   66.17  45.00  90.00  127
 30  \w     22.00  49.00   1.00    3.00    --   66.17  78.00  -0.49   27
 31  \w     23.00 151.00   1.00    3.00    --   66.17  77.00-150.00  128
 32  \w     19.00 146.00   1.00    3.00    --   66.17  45.00-180.00  127
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1376022000
_diffrn_orient_matrix_UB_12      0.0356878000
_diffrn_orient_matrix_UB_13      -0.0100933000
_diffrn_orient_matrix_UB_21      0.0470416000
_diffrn_orient_matrix_UB_22      0.0996420000
_diffrn_orient_matrix_UB_23      -0.0077308000
_diffrn_orient_matrix_UB_31      -0.0226723000
_diffrn_orient_matrix_UB_32      -0.0100083000
_diffrn_orient_matrix_UB_33      -0.1145277000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0404
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16033
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.280
_diffrn_reflns_theta_max         67.280
_diffrn_reflns_theta_min         4.219
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.816
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.34400
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.639
_exptl_crystal_description       plate
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.906
_refine_diff_density_min         -0.394
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         3630
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0402
_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^)+(0.0632P)^2^+1.3787P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1070
_refine_ls_wR_factor_ref         0.1124
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3209
_reflns_number_total             3630
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc05614j2.cif
_cod_data_source_block           sou_mnagbf4
_cod_database_code               7129190
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O Mn B F'
_shelx_estimated_absorpt_t_max   0.594
_shelx_estimated_absorpt_t_min   0.389
_reflns_odcompleteness_completeness 97.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2.a Ternary CH refined with riding coordinates:
 N1(H1)
2.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C16(H16), C17(H17),
 C18(H18), C19(H19)
;
_shelx_res_checksum              92169
_olex2_date_sample_data_collection 2020-02-07
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.655
_oxdiff_exptl_absorpt_empirical_full_min 0.540