Structural and electronic impact of fluorine in the ortho positions of triphenylphosphine and 1,2-bis(diphenylphosphino)ethane; a comparison of 2,6-difluorophenyl- with pentafluorophenyl-phosphines
Corcoran, Christopher; Fawcett, John; Friedrichs, Steffi; Holloway, John H.; Hope, Eric G.; Russell, David R.; Saunders, Graham C.; Stuart, Alison M.; Journal of the Chemical Society, Dalton Transactions  (2000) 161–; doi:10.1039/a907759f

data_7008994
_publ_section_title
;
 Structural and electronic impact of fluorine in the ortho positions of
 triphenylphosphine and 1,2-bis(diphenylphosphino)ethane; a comparison
 of 2,6-difluorophenyl- with pentafluorophenyl-phosphines
;
_journal_issue                   2
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              161
_journal_paper_doi               10.1039/a907759f
_journal_year                    2000
_chemical_formula_sum            'C37 H22 Cl F8 O P2 Rh'
_chemical_formula_weight         834.85
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.194(7)
_cell_length_b                   12.255(5)
_cell_length_c                   16.621(7)
_cell_measurement_reflns_used    51
_cell_measurement_temperature    190(2)
_cell_measurement_theta_max      12.56
_cell_measurement_theta_min      5.31
_cell_volume                     3299(2)
_computing_cell_refinement       'XSCANS (Fait, 1991)'
_computing_data_collection       'XSCANS (Fait, 1991)'
_computing_data_reduction        'XSCANS (Fait, 1991)'
_computing_molecular_graphics    'SHELXTL-pc ver5.0 (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL-pc ver5.0 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXTL-pc ver5.0 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      190(2)
_diffrn_measurement_device       'Siemens P4 diffractometer'
_diffrn_measurement_method       'omega scan'
_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  0.0223
_diffrn_reflns_av_sigmaI/netI    0.0358
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       1
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            3636
_diffrn_reflns_theta_max         25.98
_diffrn_reflns_theta_min         2.52
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.773
_exptl_absorpt_correction_T_max  0.838
_exptl_absorpt_correction_T_min  0.788
_exptl_absorpt_correction_type   'psi scan (XEMP; SHELXTL-PC)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.681
_exptl_crystal_description       block
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.405
_refine_diff_density_min         -0.414
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.059
_refine_ls_goodness_of_fit_obs   1.116
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         3161
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_restrained_S_obs      1.116
_refine_ls_R_factor_all          0.0735
_refine_ls_R_factor_obs          0.0467
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0361P)^2^+9.2697P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1067
_refine_ls_wR_factor_obs         0.0942
_reflns_number_observed          2310
_reflns_number_total             3162
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            a907759f.txt
_cod_data_source_block           9805
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0361P)^2^+9.2697P] 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^)+(0.0361P)^2^+9.2697P] 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        3298.7(24)
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               7008994