Extremely bulky secondary phosphinoamines as substituents for sterically hindered aminosilanes.
Böttcher, Tobias; Jones, Cameron; Dalton transactions (Cambridge, England : 2003) 44 (2015) 14842–14853; doi:10.1039/c5dt02504d

data_7035925
_publ_section_title
;
 Extremely bulky secondary phosphinoamines as substituents for sterically
 hindered aminosilanes.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14842
_journal_page_last               14853
_journal_paper_doi               10.1039/c5dt02504d
_journal_volume                  44
_journal_year                    2015
_chemical_formula_sum            'C47 H60 N3 P'
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_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-05-18 deposited with the CCDC.
2015-07-22 downloaded from the CCDC.
;
_cell_angle_alpha                70.230(4)
_cell_angle_beta                 73.735(4)
_cell_angle_gamma                76.194(4)
_cell_formula_units_Z            2
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_cell_length_b                   12.2272(5)
_cell_length_c                   16.8486(9)
_cell_measurement_temperature    123(2)
_cell_volume                     2067.62(19)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Apex X8'
_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  0.0314
_diffrn_reflns_av_sigmaI/netI    0.0468
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
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_diffrn_reflns_number            18998
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         3.07
_exptl_absorpt_coefficient_mu    0.101
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_exptl_absorpt_correction_T_min  0.988
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav (Blessing)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.121
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             756
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
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_refine_diff_density_max         0.506
_refine_diff_density_min         -0.501
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         7695
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0620
_refine_ls_R_factor_gt           0.0424
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0371P)^2^+0.7930P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0920
_refine_ls_wR_factor_ref         0.1030
_reflns_number_gt                5990
_reflns_number_total             7695
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt02504d2.cif
_cod_data_source_block           cj1080
_cod_depositor_comments
'Adding full bibliography for 7035922--7035934.cif.'
_cod_original_cell_volume        2067.62(18)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7035925