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_4319751
_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            'C32 H30 O3 P2'
_chemical_formula_weight         524.50
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.718(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.082(2)
_cell_length_b                   10.185(3)
_cell_length_c                   26.724(8)
_cell_measurement_reflns_used    34
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.43
_cell_measurement_theta_min      1.60
_cell_volume                     2741.1(13)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0303
_diffrn_reflns_av_sigmaI/netI    0.0419
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            8409
_diffrn_reflns_theta_full        23.50
_diffrn_reflns_theta_max         23.50
_diffrn_reflns_theta_min         2.13
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.190
_exptl_absorpt_correction_T_max  0.96338
_exptl_absorpt_correction_T_min  0.93455
_exptl_absorpt_correction_type   face-indexed
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.552
_exptl_crystal_size_mid          0.368
_exptl_crystal_size_min          0.208
_refine_diff_density_max         0.197
_refine_diff_density_min         -0.225
_refine_diff_density_rms         0.034
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment
;
 methylene and phenyl group hydrogens were given
 idealized positions [riding model]; water hydrogen
 positions were input as found in difference map
 and varied; all H's with fixed isotropic U's set
 to 1.25U[equiv] of parent atom.
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         4066
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0368
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0397P)^2^+0.5104P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0850
_refine_ls_wR_factor_ref         0.0926
_reflns_number_gt                3040
_reflns_number_total             4066
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0012367_1.cif
_cod_data_source_block           rtp002
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 
;
_cod_original_cell_volume        2741.0(13)
_cod_database_code               4319751