Chiral amino-phosphine and amido-phosphine complexes of Ir and Mg. Catalytic applications in olefin hydroamination.
Schmid, Bernhard; Frieß, Sibylle; Herrera, Alberto; Linden, Anthony; Heinemann, Frank W.; Locke, Harald; Harder, Sjoerd; Dorta, Romano; Dalton transactions (Cambridge, England : 2003) 45 (2016) 12028–12040; doi:10.1039/c6dt01146b

data_7039888
_publ_section_title
;
 Chiral amino-phosphine and amido-phosphine complexes of Ir and Mg.
 Catalytic applications in olefin hydroamination.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12028
_journal_page_last               12040
_journal_paper_doi               10.1039/c6dt01146b
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C40 H34 N2 P2, 0.5(C5 H12)'
_chemical_formula_sum            'C42.5 H40 N2 P2'
_chemical_formula_weight         640.71
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   'geom except H1N, H2N difmap'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-03-10 deposited with the CCDC.
2016-07-01 downloaded from the CCDC.
;
_cell_angle_alpha                104.466(2)
_cell_angle_beta                 107.161(2)
_cell_angle_gamma                102.209(2)
_cell_formula_units_Z            2
_cell_length_a                   10.016(2)
_cell_length_b                   12.061(3)
_cell_length_c                   16.103(4)
_cell_measurement_reflns_used    9855
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.80
_cell_measurement_theta_min      2.42
_cell_volume                     1712.1(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_publication_material  'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_structure_refinement  'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_structure_solution    'SHELXTL 6.12 (Bruker AXS, 2002)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 83.33
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker Smart APEX II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_av_sigmaI/netI    0.0290
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            42631
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    0.160
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.684
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker-AXS, 2008'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             678
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.435
_refine_diff_density_min         -0.590
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     476
_refine_ls_number_reflns         8109
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0424
_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^)+(0.0470P)^2^+1.0626P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1002
_refine_ls_wR_factor_ref         0.1091
_reflns_number_gt                6598
_reflns_number_total             8109
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6dt01146b1.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 7039888--7039891.cif.'
_cod_original_cell_volume        1712.1(6)
_cod_original_sg_symbol_Hall     -P1
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C42.50 H40 N2 P2'
_cod_database_code               7039888
_solvent_exptl_crystal_recrystallization_method 'pentane / diethyl ether'