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_7027390
_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            'C26 H46 F6 P3 Rh'
_chemical_formula_weight         668.45
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 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                 96.7910(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.8181(6)
_cell_length_b                   10.8572(3)
_cell_length_c                   29.2564(10)
_cell_measurement_temperature    223(2)
_cell_volume                     5935.5(3)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measurement_device       'Siemens SMART'
_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  0.0536
_diffrn_reflns_av_sigmaI/netI    0.0567
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            14637
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.17
_exptl_absorpt_coefficient_mu    0.789
_exptl_absorpt_correction_T_max  0.792
_exptl_absorpt_correction_T_min  0.721
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_F_000             2768
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.406
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.092
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.78(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.139
_refine_ls_goodness_of_fit_obs   1.162
_refine_ls_matrix_type           full
_refine_ls_number_parameters     660
_refine_ls_number_reflns         6885
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.155
_refine_ls_restrained_S_obs      1.162
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_obs          0.0537
_refine_ls_shift/esd_max         -0.455
_refine_ls_shift/esd_mean        0.076
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0311P)^2^+33.2706P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1142
_refine_ls_wR_factor_obs         0.1060
_reflns_number_observed          6057
_reflns_number_total             7016
_reflns_observed_criterion       2sigma(I)
_cod_data_source_file            902139fsup1.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

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^)+(0.0311P)^2^+33.2706P] 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^)+(0.0311P)^2^+33.2706P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      Cc
_cod_database_code               7027390