An Effective cis-β-Octahedral Mn(III) SALPN Catalyst for the Mukaiyama-Isayama Hydration of α,β-Unsaturated Esters
Rizzacasa, Mark A.; Donnelly, Paul Stephen; North, Andrea J.; Radjah, Natalia Caren; Ricca, Michael; Robertson, Angus Michael; White, Jonathan; Chemical Communications  (2019) –; doi:10.1039/C9CC03921J

data_7123620
_publ_section_title
;
 An Effective cis-\b-Octahedral Mn(III) SALPN Catalyst for the
 Mukaiyama-Isayama Hydration of \a,\b-Unsaturated Esters
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC03921J
_journal_year                    2019
_chemical_formula_sum            'C27 H33 Cl2 Mn N2 O6'
_chemical_formula_weight         607.39
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2019-04-05 deposited with the CCDC.    2019-06-07 downloaded from the CCDC.
;
_cell_angle_alpha                85.161(4)
_cell_angle_beta                 87.054(4)
_cell_angle_gamma                87.105(4)
_cell_formula_units_Z            2
_cell_length_a                   7.9107(4)
_cell_length_b                   11.7226(7)
_cell_length_c                   15.1375(7)
_cell_measurement_reflns_used    4280
_cell_measurement_temperature    130.01(10)
_cell_measurement_theta_max      35.5450
_cell_measurement_theta_min      3.4490
_cell_volume                     1395.40(13)
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      130.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2273
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.927
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_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  0.0360
_diffrn_reflns_av_unetI/netI     0.0656
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.927
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            19556
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.927
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.520
_diffrn_reflns_theta_min         3.183
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.708
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68498
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_description       plate
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.412
_exptl_crystal_size_mid          0.216
_exptl_crystal_size_min          0.067
_refine_diff_density_max         0.938
_refine_diff_density_min         -0.835
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         12720
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0522
_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^)+(0.0443P)^2^+0.7333P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1205
_refine_ls_wR_factor_ref         0.1391
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9604
_reflns_number_total             12720
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc03921j2.cif
_cod_data_source_block           shelx
_cod_database_code               7123620
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_usercomment     'MAR/Ricca Mn complex'
_oxdiff_exptl_absorpt_empirical_full_min 0.688
_oxdiff_exptl_absorpt_empirical_full_max 1.497
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              93443