Synthesis and Coordination Chemistry of 1,3-Bis(diphenylphosphinomethyl)benzene P,P'-Dioxide
Yun-Chou Tan; Xin-Min Gan; Jesse L. Stanchfield; Eileen N. Duesler; R. T. Paine; Inorganic Chemistry 40 (2001) 2910–2913; doi:10.1021/ic0012367

data_4319752
_publ_section_title
;
 Synthesis and Coordination Chemistry of
 1,3-Bis(diphenylphosphinomethyl)benzene P,P'-Dioxide
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2910
_journal_page_last               2913
_journal_paper_doi               10.1021/ic0012367
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C65 H60 N3 O14 P4 Y'
_chemical_formula_weight         1319.95
_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     'Patterson Map interpretation'
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                78.99(2)
_cell_angle_beta                 87.15(2)
_cell_angle_gamma                75.48(2)
_cell_formula_units_Z            2
_cell_length_a                   10.525(3)
_cell_length_b                   13.132(3)
_cell_length_c                   25.184(5)
_cell_measurement_reflns_used    72
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.332
_cell_measurement_theta_min      1.666
_cell_volume                     3307.6(14)
_computing_cell_refinement       'Siemens XSCANS, 1991'
_computing_data_collection       'Siemens XSCANS, 1991'
_computing_data_reduction        'Siemens XSCANS, 1991'
_computing_molecular_graphics    'Siemens SHELXTL Version 5, 1994'
_computing_publication_material  'Siemens SHELXTL Version 5, 1994'
_computing_structure_refinement  'Siemens SHELXTL Version 5, 1994'
_computing_structure_solution    'Siemens SHELXTL Version 5, 1994'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0890
_diffrn_reflns_av_sigmaI/netI    0.2680
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            22925
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.96
_diffrn_standards_decay_%        8.50
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.042
_exptl_absorpt_correction_T_max  0.965
_exptl_absorpt_correction_T_min  0.861
_exptl_absorpt_correction_type   'empirical via \y scans'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             1364
_exptl_crystal_size_max          0.345
_exptl_crystal_size_mid          0.345
_exptl_crystal_size_min          0.276
_refine_diff_density_max         0.886
_refine_diff_density_min         -0.447
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.152
_refine_ls_goodness_of_fit_obs   2.081
_refine_ls_hydrogen_treatment
;
 The hydrogen on O16 was fixed in a reasonable position located in a
 difference map. The hydrogens on O17 and O17' were not seen in the
 difference maps; so the hydrogens on O17,O17' and C66 were not included
 in the refinements; all other hydrogens were included in idealized
 positions [riding model]; all hydrogens were refined with fixed isotropic
 U's set to 1.25U(equiv) or 1.25U(isotropic) of parent atom.
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     763
_refine_ls_number_reflns         11600
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.166
_refine_ls_restrained_S_obs      2.106
_refine_ls_R_factor_all          0.1782
_refine_ls_R_factor_obs          0.0650
_refine_ls_shift/esd_max         0.185
_refine_ls_shift/esd_mean        0.028
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1599
_refine_ls_wR_factor_obs         0.1514
_reflns_number_observed          3715
_reflns_number_total             11600
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0012367_2.cif
_cod_data_source_block           rtp97ga
_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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4319752