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_7012019
_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            'C74 H86 N5 Nd O19 P4'
_chemical_formula_weight         1617.60
_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                86.4940(10)
_cell_angle_beta                 79.8130(10)
_cell_angle_gamma                83.3800(10)
_cell_formula_units_Z            2
_cell_length_a                   13.2909(8)
_cell_length_b                   14.9667(9)
_cell_length_c                   20.0288(11)
_cell_measurement_temperature    293(2)
_cell_volume                     3891.8(4)
_computing_cell_refinement       'SMART V4.0 (Bruker/Siemens)'
_computing_data_collection       'SMART V4.0 (Bruker/Siemens)'
_computing_data_reduction        'SAINT V5.1 (Bruker/Siemens)'
_computing_molecular_graphics    'SHELXTL V5.0 (Siemens, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean '10 s/frame'
_diffrn_measured_fraction_theta_full 0.580
_diffrn_measured_fraction_theta_max 0.580
_diffrn_measurement_device_type  'Bruker/Siemens Smart/P4 CCD'
_diffrn_measurement_method       hemisphere
_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  0.0276
_diffrn_reflns_av_sigmaI/netI    0.0361
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            22883
_diffrn_reflns_theta_full        29.02
_diffrn_reflns_theta_max         29.02
_diffrn_reflns_theta_min         1.37
_exptl_absorpt_coefficient_mu    0.820
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.828143
_exptl_absorpt_correction_type   'SADABS correction'
_exptl_crystal_colour            'pale blue'
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'long plate'
_exptl_crystal_F_000             1674
_exptl_crystal_size_max          1.15
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.130
_refine_diff_density_min         -0.692
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     821
_refine_ls_number_reflns         12021
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0457
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0829P)^2^+5.0429P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1292
_refine_ls_wR_factor_ref         0.1363
_reflns_number_gt                10188
_reflns_number_total             12021
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b206782j.txt
_cod_data_source_block           sad1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7012019