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_7129189
_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         'C22 H14 Br Mn N2 O4, 1[C4H8O]'
_chemical_formula_sum            'C22 H14 Br Mn N2 O4'
_chemical_formula_weight         505.20
_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             2021-07-16
_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                 94.232(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9430(3)
_cell_length_b                   12.3084(3)
_cell_length_c                   17.5419(4)
_cell_measurement_reflns_used    3573
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      24.9920
_cell_measurement_theta_min      2.1070
_cell_volume                     2356.29(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33c (release 11-04-2014 CrysAlis171 .NET)
(compiled Apr 11 2014,15:12:41)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33c (release 11-04-2014 CrysAlis171 .NET)
(compiled Apr 11 2014,15:12:41)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33c (release 11-04-2014 CrysAlis171 .NET)
(compiled Apr 11 2014,15:12:41)
;
_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  (Sheldrick, 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 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
  1 omega  -50.00   65.00   1.0000   14.3450
omega____ theta____ kappa____ phi______ frames
    -       27.0898  -57.0000    0.0000 115

  2 omega  -23.00  101.00   1.0000   14.3450
omega____ theta____ kappa____ phi______ frames
    -       27.0898   38.0000  -60.0000 124
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0516712000
_diffrn_orient_matrix_UB_12      -0.0295185000
_diffrn_orient_matrix_UB_13      -0.0107153000
_diffrn_orient_matrix_UB_21      -0.0353019000
_diffrn_orient_matrix_UB_22      -0.0212895000
_diffrn_orient_matrix_UB_23      -0.0321149000
_diffrn_orient_matrix_UB_31      0.0173618000
_diffrn_orient_matrix_UB_32      0.0446956000
_diffrn_orient_matrix_UB_33      -0.0223488000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0236
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            7041
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.023
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.283
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73222
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33c (release 11-04-2014 CrysAlis171 .NET)
(compiled Apr 11 2014,15:12:41)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_description       block
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.616
_refine_diff_density_min         -0.523
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         4132
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0338
_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^)+(0.0435P)^2^+1.2470P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0857
_refine_ls_wR_factor_ref         0.0894
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3612
_reflns_number_total             4132
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc05614j2.cif
_cod_data_source_block           mnbr1
_cod_database_code               7129189
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O Mn Br'
_shelx_estimated_absorpt_t_max   0.804
_shelx_estimated_absorpt_t_min   0.726
_reflns_odcompleteness_completeness 92.36
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.63
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2A), C3(H3), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C16(H16), C17(H17),
  C18(H18), C19(H19)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 166 electrons were 
found in a volume of 498\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1[C4H8O] per Formula Unit 
which account for 160 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              7357
_shelx_fab_checksum              92766
_olex2_date_sample_data_collection 2018-03-13
_olex2_submission_special_instructions 'No special instructions were received'