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_7012016
_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            'C78 H88 N5 Nd O16 P4'
_chemical_formula_weight         1619.65
_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                89.170(10)
_cell_angle_beta                 77.158(13)
_cell_angle_gamma                64.186(11)
_cell_formula_units_Z            4
_cell_length_a                   16.905(3)
_cell_length_b                   18.322(3)
_cell_length_c                   31.301(5)
_cell_measurement_reflns_used    51
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11.10
_cell_measurement_theta_min      2.49
_cell_volume                     8472(3)
_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 0.978
_diffrn_measured_fraction_theta_max 0.978
_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  0.1125
_diffrn_reflns_av_sigmaI/netI    0.1682
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            33010
_diffrn_reflns_theta_full        21.50
_diffrn_reflns_theta_max         21.50
_diffrn_reflns_theta_min         1.63
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.751
_exptl_absorpt_correction_T_max  0.9690
_exptl_absorpt_correction_T_min  0.7510
_exptl_absorpt_correction_type   'empirical psi-scans'
_exptl_crystal_colour            pale_blue
_exptl_crystal_density_diffrn    1.270
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3356
_exptl_crystal_size_max          0.356
_exptl_crystal_size_mid          0.254
_exptl_crystal_size_min          0.138
_refine_diff_density_max         1.270
_refine_diff_density_min         -1.502
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     801
_refine_ls_number_reflns         19037
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.1928
_refine_ls_R_factor_gt           0.1060
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1900P)^2^+12.5000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2867
_refine_ls_wR_factor_ref         0.3519
_reflns_number_gt                9591
_reflns_number_total             19037
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b206782j.txt
_cod_data_source_block           rtp009
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        8472(2)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7012016