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_7123621
_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            'C32 H47 Mn N2 O7.5'
_chemical_formula_weight         634.65
_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'
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_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-04-05 deposited with the CCDC.    2019-06-07 downloaded from the CCDC.
;
_cell_angle_alpha                81.588(10)
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_cell_angle_gamma                85.486(12)
_cell_formula_units_Z            2
_cell_length_a                   10.2610(16)
_cell_length_b                   10.8556(15)
_cell_length_c                   14.6929(15)
_cell_measurement_reflns_used    970
_cell_measurement_temperature    130.01(10)
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_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
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_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
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_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      130.01(10)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.842
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_unetI/netI     0.0845
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.842
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            7657
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.842
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.074
_diffrn_reflns_theta_min         3.165
_exptl_absorpt_coefficient_mu    0.460
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58041
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_description       rod
_exptl_crystal_F_000             676
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.296
_refine_diff_density_min         -1.022
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         7657
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.1300
_refine_ls_R_factor_gt           0.0757
_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^)+(0.1545P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2068
_refine_ls_wR_factor_ref         0.2389
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4611
_reflns_number_total             7657
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc03921j2.cif
_cod_data_source_block           shelx_CCDC1
_cod_original_formula_sum        'C32 H47 Mn N2 O7.50'
_cod_database_code               7123621
_shelx_shelxl_version_number     2014/7
_cell_oxdiff_twin_number         2
_shelx_res_checksum              96577