Insertion of Carbon Fragments into P(III)-N Bonds in Aminophosphines and Aminobis(phosphines): Synthesis, Reactivity, and Coordination Chemistry of Resulting Phosphine Oxide Derivatives. Crystal and Molecular Structures of (Ph2P(O)CH2)2NR (R = Me,nPr,nBu), Ph2P(O)CH(OH)nPr, and cis-[MoO2Cl2{(Ph2P(O)CH2)2NEt-κO,κO}]
Srinivasan Priya; Maravanji S. Balakrishna; Joel T. Mague; Shaikh M. Mobin; Inorganic Chemistry 42 (2003) 1272–1281; doi:10.1021/ic026118t

data_4313188
_publ_section_title
;
 Insertion of Carbon Fragments into P(III)-N Bonds in Aminophosphines and
 Aminobis(phosphines): Synthesis, Reactivity, and Coordination Chemistry
 of Resulting Phosphine Oxide Derivatives. Crystal and Molecular
 Structures of (Ph2P(O)CH2)2NR (R = Me,nPr,nBu), Ph2P(O)CH(OH)nPr, and
 cis-[MoO2Cl2{(Ph2P(O)CH2)2NEt-\kO,\kO}]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1272
_journal_page_last               1281
_journal_paper_doi               10.1021/ic026118t
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C30 H33 N O2 P2'
_chemical_formula_weight         501.51
_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                85.72(3)
_cell_angle_beta                 89.53(3)
_cell_angle_gamma                89.81(3)
_cell_formula_units_Z            2
_cell_length_a                   8.0530(16)
_cell_length_b                   10.287(2)
_cell_length_c                   16.264(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1343.5(5)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_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  0.0092
_diffrn_reflns_av_sigmaI/netI    0.0175
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            5113
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.26
_exptl_absorpt_coefficient_mu    0.189
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             532
_refine_diff_density_max         0.377
_refine_diff_density_min         -0.242
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         4741
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0395
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0439P)^2^+0.7530P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1045
_refine_ls_wR_factor_ref         0.1122
_reflns_number_gt                4007
_reflns_number_total             4741
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic026118t_s3.cif
_cod_data_source_block           msb106
_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 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4313188