First Representative of Optically Active P-l-Menthyl-Substituted (Aminomethyl)phosphine and Its Borane and Metal Complexes
Svetlana N. Ignatieva; Anna S. Balueva; Andrey A. Karasik; Shamil K. Latypov; Anna G. Nikonova; Olga E. Naumova; Peter Lönnecke; Evamarie Hey-Hawkins; Oleg G. Sinyashin; Inorganic Chemistry 49 (2010) 5407–5412; doi:10.1021/ic902564n

data_4315869
_publ_section_title
;
 First Representative of Optically Active P-l-Menthyl-Substituted
 (Aminomethyl)phosphine and Its Borane and Metal Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5407
_journal_page_last               5412
_journal_paper_doi               10.1021/ic902564n
_journal_volume                  49
_journal_year                    2010
_chemical_absolute_configuration rmad
_chemical_formula_sum            'C40 H64 Cl6 N2 P2 Pt'
_chemical_formula_weight         1042.66
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2007-10-10T10:54:36-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.10170(10)
_cell_length_b                   21.4564(2)
_cell_length_c                   25.1560(2)
_cell_measurement_reflns_used    92476
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      32.2918
_cell_measurement_theta_min      2.5974
_cell_volume                     4372.95(8)
_computing_cell_refinement
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
        (compiled May  8 2007,13:10:02)
;
_computing_data_collection
;
        CrysAlis CCD, Oxford Diffraction Ltd.,
        Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
        (compiled May  8 2007,13:10:02)
;
_computing_data_reduction
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
        (compiled May  8 2007,13:10:02)
;
_computing_molecular_graphics    'ORTEP3 for Windows (L. J. Farrugia, 1997)'
_computing_publication_material  'WINGX  (L.J. Farrugia,1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Giacovazzo 1993)'
_diffrn_ambient_temperature      130(2)
_diffrn_detector_area_resol_mean 16.356
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'ccd Xcalibur S'
_diffrn_measurement_method       '\w- amd \f-scans'
_diffrn_orient_matrix_UB_11      0.0125734668
_diffrn_orient_matrix_UB_12      -0.0128276557
_diffrn_orient_matrix_UB_13      -0.025632019
_diffrn_orient_matrix_UB_21      0.0212010663
_diffrn_orient_matrix_UB_22      -0.0289795662
_diffrn_orient_matrix_UB_23      0.0116097426
_diffrn_orient_matrix_UB_31      -0.0838517873
_diffrn_orient_matrix_UB_32      -0.0092738299
_diffrn_orient_matrix_UB_33      -0.0009651859
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_av_unetI/netI     0.0182
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            142867
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         2.61
_exptl_absorpt_coefficient_mu    3.68
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.64023
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
        (compiled May  8 2007,13:10:02)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.584
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.2
_refine_diff_density_min         -0.814
_refine_diff_density_rms         0.077
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.014(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         13363
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0199
_refine_ls_R_factor_gt           0.0176
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0163P)^2^+2.0700P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0367
_refine_ls_wR_factor_ref         0.038
_reflns_number_gt                12776
_reflns_number_total             13363
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic902564n_si_001.cif
_cod_data_source_block           x0314fin
_cod_database_code               4315869