Yttrium-Catalyzed Amine‒Silane Dehydrocoupling: Extended Reaction Scope with a Phosphorus-Based Ligand
Nako, Adi E.; Chen, Wenyi; White, Andrew J. P.; Crimmin, Mark R.; Organometallics 34 (2015) 4369–; doi:10.1021/acs.organomet.5b00607

data_4087801
_publ_section_title
;
 Yttrium-Catalyzed Amine--Silane Dehydrocoupling: Extended Reaction Scope
 with a Phosphorus-Based Ligand
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              4369
_journal_paper_doi               10.1021/acs.organomet.5b00607
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C35 H63 N3 P Si4 Y'
_chemical_formula_sum            'C35 H63 N3 P Si4 Y'
_chemical_formula_weight         758.12
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL
_cell_angle_alpha                90
_cell_angle_beta                 100.920(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.1540(6)
_cell_length_b                   12.9620(5)
_cell_length_c                   22.1453(8)
_cell_measurement_reflns_used    5421
_cell_measurement_temperature    173
_cell_measurement_theta_max      26.9530
_cell_measurement_theta_min      2.6240
_cell_volume                     4271.2(3)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'CIFTAB-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 16.0382
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.802
_diffrn_measurement_device_type  'Agilent Xcalibur 3 E'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_unetI/netI     0.0579
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.802
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15137
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.802
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.310
_diffrn_reflns_theta_min         2.389
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.541
_exptl_absorpt_correction_T_max  0.872
_exptl_absorpt_correction_T_min  0.760
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33a (release 28-03-2014 CrysAlis171 .NET)
(compiled Mar 28 2014,12:25:20)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.179
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.366
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         8535
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0394
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0366P)^2^+0.9518P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0792
_refine_ls_wR_factor_ref         0.0876
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6459
_reflns_number_total             8535
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00607_si_003.cif
_cod_data_source_block           3b
_cod_original_cell_volume        4271.1(3)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4087801
_shelxl_version_number           2013-4