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_4319753
_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            'C64.5 H58 Er N3 O13.5 P4'
_chemical_formula_weight         1382.28
_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                78.85(2)
_cell_angle_beta                 87.33(1)
_cell_angle_gamma                75.59(2)
_cell_formula_units_Z            2
_cell_length_a                   10.507(2)
_cell_length_b                   13.098(3)
_cell_length_c                   25.151(5)
_cell_measurement_reflns_used    52
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.50
_cell_measurement_theta_min      1.64
_cell_volume                     3289.1(12)
_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  0.0758
_diffrn_reflns_av_sigmaI/netI    0.1699
_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            23138
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         1.96
_diffrn_standards_decay_%        11.14
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.436
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_correction_T_min  0.767
_exptl_absorpt_correction_type   'empirical via \y scans'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             1404
_exptl_crystal_size_max          0.378
_exptl_crystal_size_mid          0.368
_exptl_crystal_size_min          0.138
_refine_diff_density_max         1.280
_refine_diff_density_min         -0.522
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.995
_refine_ls_goodness_of_fit_obs   1.358
_refine_ls_hydrogen_treatment
;
 riding model for all hydrogens except disordered H's; the methanolic
 hydrogen was fixed in positions found in difference maps and all
 hydrogen atoms had fixed isotropic U's set to 1.25U(equivalent, for ordered
 hydrogens) or 1.25U(isotropic, for disordered hydrogens) of their parent
 atoms.
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     755
_refine_ls_number_reflns         11573
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.067
_refine_ls_restrained_S_obs      1.369
_refine_ls_R_factor_all          0.1055
_refine_ls_R_factor_obs          0.0548
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1387
_refine_ls_wR_factor_obs         0.1232
_reflns_number_observed          5884
_reflns_number_total             11574
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0012367_3.cif
_cod_data_source_block           rtp97f
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0350P)^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^)+(0.0350P)^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_original_formula_sum        'C64.50 H58 Er N3 O13.50 P4'
_cod_database_code               4319753