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_4080110
_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         '(C66 H102 N9 Y)(1), (C4 H10 O)(0.5)'
_chemical_formula_sum            'C68 H107 N9 O0.5 Y'
_chemical_formula_weight         1147.54
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.9550(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.4154(3)
_cell_length_b                   22.0265(3)
_cell_length_c                   21.5060(4)
_cell_measurement_reflns_used    9255
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      70.34
_cell_measurement_theta_min      2.89
_cell_volume                     6762.9(2)
_computing_cell_refinement       'Bruker SAINT v6.22'
_computing_data_collection       'Bruker SMART v5.625'
_computing_data_reduction        'Bruker SAINT v6.622'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  \w-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0485
_diffrn_reflns_av_sigmaI/netI    0.0225
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            115671
_diffrn_reflns_theta_full        70.64
_diffrn_reflns_theta_max         70.64
_diffrn_reflns_theta_min         2.89
_exptl_absorpt_coefficient_mu    1.549
_exptl_absorpt_correction_T_max  0.753
_exptl_absorpt_correction_T_min  0.664
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.127
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2484
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.717
_refine_diff_density_min         -0.915
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     790
_refine_ls_number_reflns         12801
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0841
_refine_ls_R_factor_gt           0.0724
_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^)+(0.1398P)^2^+9.8295P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2152
_refine_ls_wR_factor_ref         0.2296
_reflns_number_gt                10701
_reflns_number_total             12801
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300807k_si_003.cif
_cod_data_source_block           Y[CyNC(DMBA)NCy]3_(3)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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      P2(1)/n
_cod_original_formula_sum        'C68 H107 N9 O0.50 Y'
_cod_database_code               4080110