Synthesis of η1-α-Phosphinocarbene Complexes of Manganese and Mechanistic Insight into Their Base-Induced Transformations
Valyaev, Dmitry A.; Lugan, Noël; Lavigne, Guy; Ustynyuk, Nikolai A.; Organometallics 30 (2011) 2318–; doi:10.1021/om2000772

data_4064397
_publ_section_title
;
 Synthesis of \h1-\a-Phosphinocarbene Complexes of Manganese and
 Mechanistic Insight into Their Base-Induced Transformations
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              2318
_journal_paper_doi               10.1021/om2000772
_journal_volume                  30
_journal_year                    2011
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C18 H20 Mn O2 P'
_chemical_formula_sum            'C18 H20 Mn O2 P'
_chemical_formula_weight         354.25
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2010-05-09T11:14:15-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90.0
_cell_angle_beta                 103.52(3)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   13.045(4)
_cell_length_b                   10.2333(17)
_cell_length_c                   13.172(4)
_cell_measurement_reflns_used    6162
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      32.0739
_cell_measurement_theta_min      2.8069
_cell_measurement_wavelength     0.71073
_cell_volume                     1709.6(8)
_computing_cell_refinement
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET)
        (compiled Apr 27 2007,17:53:11)
;
_computing_data_collection
;
        CrysAlis CCD, Oxford Diffraction Ltd.,
        Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET)
        (compiled Apr 27 2007,17:53:11)
;
_computing_data_reduction
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET)
        (compiled Apr 27 2007,17:53:11)
;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      160(2)
_diffrn_detector_area_resol_mean 8.2632
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Xcalibur Oxford Diffraction'
_diffrn_measurement_method       \f
_diffrn_orient_matrix_UB_11      -0.0332978439
_diffrn_orient_matrix_UB_12      -0.0459064293
_diffrn_orient_matrix_UB_13      -0.032249349
_diffrn_orient_matrix_UB_21      0.0258016081
_diffrn_orient_matrix_UB_22      -0.0517715389
_diffrn_orient_matrix_UB_23      0.0318242588
_diffrn_orient_matrix_UB_31      -0.0367242201
_diffrn_orient_matrix_UB_32      0.0052173436
_diffrn_orient_matrix_UB_33      0.0321656018
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0492
_diffrn_reflns_av_sigmaI/netI    0.0452
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12778
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.81
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.869
_exptl_absorpt_correction_T_max  0.920
_exptl_absorpt_correction_T_min  0.774
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET)
        (compiled Apr 27 2007,17:53:11)
        Empirical absorption correction using spherical harmonics,
        implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.067
_refine_diff_density_min         -0.358
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     207
_refine_ls_number_reflns         3488
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0467
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0772P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1295
_refine_ls_wR_factor_ref         0.1466
_reflns_number_gt                2499
_reflns_number_total             3488
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om2000772_si_002.cif
_cod_data_source_block           complex_3b
_cod_database_code               4064397