A new synthetic route to ligands of the general composition R2PCH2ER′2 (E = P, As) and some rhodium complexes derived thereof
Wolf, Justin; Manger, Matthias; Schmidt, Ulrich; Fries, Guido; Barth, Dietmar; Weberndörfer, Birgit; Vicic, David A.; Jones, William D.; Werner, Helmut; Journal of the Chemical Society, Dalton Transactions  (1999) 1867–; doi:10.1039/a902139f

data_7027391
_publ_contact_author
;
        Prof. Dr. Helmut Werner
        Institut f\"ur Anorganische Chemie
        Universit\"at W\"urzburg
        Am Hubland
        D-97074 W\"urzburg
        Deutschland
;
_publ_section_title
;
 A new synthetic route to ligands of the general composition
 R2PCH2ER&#x2032;2 (E&#x2005;=&#x2005;P, As) and some rhodium complexes
 derived thereof
;
_journal_issue                   11
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1867
_journal_paper_doi               10.1039/a902139f
_journal_year                    1999
_chemical_formula_sum            'C33 H62 As P'
_chemical_formula_weight         564.72
_chemical_melting_point          340.15
_space_group_IT_number           152
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      152
_symmetry_space_group_name_Hall  'P 31 2"'
_symmetry_space_group_name_H-M   'P 31 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   10.0640(4)
_cell_length_b                   10.0640(4)
_cell_length_c                   57.716(4)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.1
_cell_measurement_theta_min      2.34
_cell_volume                     5062.5(5)
_computing_cell_refinement       'IPDS (STOE)'
_computing_data_collection       'IPDS (STOE)'
_computing_data_reduction        'IPDS (STOE)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'IPDS (STOE)'
_diffrn_measurement_method       'PSI scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0430
_diffrn_reflns_av_sigmaI/netI    0.0853
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       66
_diffrn_reflns_limit_l_min       -58
_diffrn_reflns_number            10185
_diffrn_reflns_theta_max         24.17
_diffrn_reflns_theta_min         2.34
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.071
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.111
_exptl_crystal_description       prism
_exptl_crystal_F_000             1848
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.373
_refine_diff_density_min         -0.410
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.039(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.927
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         4857
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.898
_refine_ls_restrained_S_obs      1.016
_refine_ls_R_factor_all          0.0729
_refine_ls_R_factor_gt           0.0418
_refine_ls_shift/esd_mean        0.000
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0377P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0955
_refine_ls_wR_factor_ref         0.0854
_reflns_number_gt                3469
_reflns_number_total             5402
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            902139fsup1.cif
_cod_data_source_block           mm2wb
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '67_C' was changed to '340.15' - it
was converted from degrees Celsius(C) to Kelvins(K).

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0377P)^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^)+(0.0377P)^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_cell_volume        5062.5(4)
_cod_original_sg_symbol_H-M      P3121
_cod_database_code               7027391