Mn(i) organometallics containing the iPr2P(CH2)2PiPr2 ligand for the catalytic hydration of aromatic nitriles
Garduño, Jorge A.; Arévalo, Alma; Flores-Alamo, Marcos; García, Juventino J.; Catalysis Science & Technology 8 (2018) 2606–; doi:10.1039/C8CY00416A

data_1549242
_publ_section_title
;
 Mn(i) organometallics containing the iPr2P(CH2)2PiPr2 ligand for the
 catalytic hydration of aromatic nitriles
;
_journal_issue                   10
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              2606
_journal_paper_doi               10.1039/C8CY00416A
_journal_volume                  8
_journal_year                    2018
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C18 H32 F3 Mn O6 P2 S'
_chemical_formula_sum            'C18 H32 F3 Mn O6 P2 S'
_chemical_formula_weight         550.37
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_creation_date             2018-01-19T10:33:28-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2018-01-19 deposited with the CCDC.
2018-04-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.6949(6)
_cell_length_b                   13.9549(9)
_cell_length_c                   19.9508(15)
_cell_measurement_reflns_used    1374
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      26.031
_cell_measurement_theta_min      3.869
_cell_volume                     2420.8(3)
_computing_cell_refinement
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
        (compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
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        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
        (compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
        (compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics
;
          'Ortep-3 for Windows (Farrugia, 1997)'
      L. J. Farrugia, J. Appl. Crystallogr., 1997, 30, 565.
;
_computing_publication_material
;    
        'WinGX publication routines (Farrugia, 1999)'                 
    L. J. Farrugia, J. Appl. Crystallogr., 1999, 32, 837-838.
;
_computing_structure_refinement
;
      'SHELXS-2014 (Sheldrick, 2015)'
      Sheldrick, G. M. (2015). Acta Cryst. C71, 3--8.
;
_computing_structure_solution
;
      'SHELXS-2014 (Sheldrick, 2015)'
      Sheldrick, G. M. (2015). Acta Cryst. A71, 3--8.
;
_diffrn_ambient_temperature      130(2)
_diffrn_detector_area_resol_mean 10.4685
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0157444
_diffrn_orient_matrix_UB_12      0.0044835
_diffrn_orient_matrix_UB_13      0.0346634
_diffrn_orient_matrix_UB_21      -0.0796262
_diffrn_orient_matrix_UB_22      -0.0049143
_diffrn_orient_matrix_UB_23      -0.0065855
_diffrn_orient_matrix_UB_31      0.006369
_diffrn_orient_matrix_UB_32      -0.0503027
_diffrn_orient_matrix_UB_33      0.0038266
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1015
_diffrn_reflns_av_unetI/netI     0.1649
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            6815
_diffrn_reflns_point_group_measured_fraction_full 0.922
_diffrn_reflns_point_group_measured_fraction_max 0.922
_diffrn_reflns_theta_full        25.347
_diffrn_reflns_theta_max         25.347
_diffrn_reflns_theta_min         3.394
_exptl_absorpt_coefficient_mu    0.818
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_correction_T_min  0.885
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
        (compiled Aug  2 2013,16:46:58)
Analytical numeric absorption correction using a multifaceted crystal
                        model based on expressions derived by R.C. Clark & J.S.
        (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.51
_exptl_crystal_description       plate
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.769
_refine_diff_density_min         -0.549
_refine_diff_density_rms         0.121
_refine_ls_abs_structure_details
;
 Flack x determined using 785 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.03(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         4087
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.1202
_refine_ls_R_factor_gt           0.0766
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0870P)^2^+0.3322P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1661
_refine_ls_wR_factor_ref         0.197
_reflns_Friedel_coverage         0.621
_reflns_Friedel_fraction_full    0.824
_reflns_Friedel_fraction_max     0.823
_reflns_number_gt                2832
_reflns_number_total             4087
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cy00416a2.cif
_cod_data_source_block           2
_cod_depositor_comments          'Adding full bibliography for 1549242.cif.'
_cod_database_code               1549242
_shelx_estimated_absorpt_t_min   0.736
_shelx_estimated_absorpt_t_max   0.976