Synthesis and coordination chemistry of arene soluble 4-alkyl-2,6-bis[(diphenylphosphino)methyl]pyridine N,P,P'-trioxide ligands
Xin-Min Gan; Robert T. Paine; Eileen N. Duesler; Heinrich Nöth; Dalton Trans.  (2003) 153–159; doi:10.1039/b206782j

data_7012018
_publ_section_title
;
 Synthesis and coordination chemistry of arene soluble
 4-alkyl-2,6-bis[(diphenylphosphino)methyl]pyridine N,P,P'-trioxide
 ligands
;
_journal_issue                   1
_journal_name_full               'Dalton Trans.'
_journal_page_first              153
_journal_page_last               159
_journal_paper_doi               10.1039/b206782j
_journal_year                    2003
_chemical_formula_sum            'C132 H127 N13 Nd3 O40.5 P8'
_chemical_formula_weight         3223.95
_chemical_name_systematic
; 
? 
;
_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                79.42(2)
_cell_angle_beta                 76.79(3)
_cell_angle_gamma                71.69(3)
_cell_formula_units_Z            2
_cell_length_a                   17.830(7)
_cell_length_b                   17.959(6)
_cell_length_c                   25.691(8)
_cell_measurement_reflns_used    53
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      10.47
_cell_measurement_theta_min      2.23
_cell_volume                     7547(5)
_computing_cell_refinement       'Bruker, XSCANS'
_computing_data_collection       'Bruker, XSCANS'
_computing_data_reduction        'Bruker, XSCANS'
_computing_molecular_graphics    'Bruker, Shelxtl NT 5.0'
_computing_publication_material  'Bruker, Shelxtl NT 5.0'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.371
_diffrn_measured_fraction_theta_max 0.371
_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  0.0677
_diffrn_reflns_av_sigmaI/netI    0.0630
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            55366
_diffrn_reflns_theta_full        31.80
_diffrn_reflns_theta_max         31.80
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    1.180
_exptl_absorpt_correction_T_max  0.78745
_exptl_absorpt_correction_T_min  0.57430
_exptl_absorpt_correction_type   'Gaussian Face-indexed'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3268
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.345
_refine_diff_density_min         -1.279
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1503
_refine_ls_number_reflns         19135
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.1126
_refine_ls_R_factor_gt           0.0839
_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^)+(0.0996P)^2^+86.7152P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2388
_refine_ls_wR_factor_ref         0.2579
_reflns_number_gt                14024
_reflns_number_total             19135
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b206782j.txt
_cod_data_source_block           rtp012t
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C132 H127 N13 Nd3 O40.50 P8'
_cod_database_code               7012018