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_4087799
_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_absolute_configuration ad
_chemical_formula_moiety         'C37 H71 N3 P Si6 Y'
_chemical_formula_sum            'C37 H71 N3 P Si6 Y'
_chemical_formula_weight         846.39
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21 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                 97.0732(19)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.2125(3)
_cell_length_b                   16.1022(3)
_cell_length_c                   12.5748(2)
_cell_measurement_reflns_used    6992
_cell_measurement_temperature    173
_cell_measurement_theta_max      29.5220
_cell_measurement_theta_min      3.0049
_cell_volume                     2453.99(9)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd'
_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      173
_diffrn_detector_area_resol_mean 15.9825
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.858
_diffrn_measurement_device_type  'OD Xcalibur 3'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_av_sigmaI/netI    0.0474
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            20447
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         29.59
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    1.394
_exptl_absorpt_correction_T_max  0.857
_exptl_absorpt_correction_T_min  0.773
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) 
(compiled Jan 23 2012,18:06:46) 
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) 
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.145
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.319
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details
'Flack H D (1983), Acta Cryst. A39, 876-881, 4195 Friedel pairs'
_refine_ls_abs_structure_Flack   0.051(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         10306
_refine_ls_number_restraints     50
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0367
_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^)+(0.0380P)^2^+0.3578P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0746
_refine_ls_wR_factor_ref         0.0792
_reflns_number_gt                8946
_reflns_number_total             10306
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5b00607_si_003.cif
_cod_data_source_block           2.CH2PPh3
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               4087799