Insertion Reactions and Catalytic Hydrophosphination of Heterocumulenes using α-MetalatedN,N-Dimethylbenzylamine Rare-Earth-Metal Complexes
Behrle, Andrew C.; Schmidt, Joseph A. R.; Organometallics 32 (2013) 1141–1149; doi:10.1021/om300807k

data_4080111
_publ_section_title
;
 Insertion Reactions and Catalytic Hydrophosphination of Heterocumulenes
 using \a-MetalatedN,N-Dimethylbenzylamine Rare-Earth-Metal Complexes
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1141
_journal_page_last               1149
_journal_paper_doi               10.1021/om300807k
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C34 H54 N5 Si2 Y'
_chemical_formula_sum            'C34 H54 N5 Si2 Y'
_chemical_formula_weight         677.91
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                98.193(1)
_cell_angle_beta                 96.863(1)
_cell_angle_gamma                108.486(1)
_cell_formula_units_Z            2
_cell_length_a                   9.1050(2)
_cell_length_b                   11.1607(3)
_cell_length_c                   18.8762(5)
_cell_measurement_reflns_used    7456
_cell_measurement_temperature    120
_cell_measurement_theta_max      67.87
_cell_measurement_theta_min      2.40
_cell_volume                     1772.70(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.917
_diffrn_measured_fraction_theta_max 0.869
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0449
_diffrn_reflns_av_sigmaI/netI    0.0679
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            9943
_diffrn_reflns_theta_full        60.00
_diffrn_reflns_theta_max         67.86
_diffrn_reflns_theta_min         2.40
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.181
_exptl_absorpt_correction_T_max  0.7530
_exptl_absorpt_correction_T_min  0.5664
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.270
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.722
_refine_diff_density_min         -0.897
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     387
_refine_ls_number_reflns         5603
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0458
_refine_ls_shift/su_max          0.095
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0755P)^2^+1.9551P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1256
_refine_ls_wR_factor_ref         0.1275
_reflns_number_gt                5333
_reflns_number_total             5603
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300807k_si_003.cif
_cod_data_source_block           Y(DMBA)2(TMSNC(DMBA)NTMS)_4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4080111