Carbon‒fluorine bond activation in the reactions between 1,2-bis[bis(2,6-difluorophenyl)phosphino]ethane and [{MCl(μ-Cl)(η5-C5Me5)}2] (M = Rh or Ir)
Fawcett, John; Friedrichs, Steffi; Holloway, John H.; Hope, Eric G.; McKee, Vickie; Nieuwenhuyzen, Mark; Russell, David R.; Saunders, Graham C.; Journal of the Chemical Society, Dalton Transactions  (1998) 1477–; doi:10.1039/a800515j

data_7028180
_publ_section_title
;
 Carbon--fluorine bond activation in the reactions between
 1,2-bis[bis(2,6-difluorophenyl)phosphino]ethane and
 [{MCl(\m-Cl)(\h5-C5Me5)}2] (M&#x2005;=&#x2005;Rh or Ir)
;
_journal_issue                   9
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1477
_journal_paper_doi               10.1039/a800515j
_journal_year                    1998
_chemical_formula_sum            'C52 H46 Cl4 F20 Ir2 O2 P2'
_chemical_formula_weight         1671.03
_chemical_name_systematic
; 
 ? 
;
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                86.30(2)
_cell_angle_beta                 79.36(2)
_cell_angle_gamma                78.87(2)
_cell_formula_units_Z            2
_cell_length_a                   12.149(2)
_cell_length_b                   12.650(3)
_cell_length_c                   19.663(4)
_cell_measurement_reflns_used    41
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.54
_cell_measurement_theta_min      3.77
_cell_volume                     2912.8(11)
_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      153(2)
_diffrn_measurement_device       'Siemens 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  0.0240
_diffrn_reflns_av_sigmaI/netI    0.0428
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            10772
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.11
_diffrn_standards_decay_%        4.99
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.906
_exptl_absorpt_correction_T_max  0.9081
_exptl_absorpt_correction_T_min  0.6313
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.905
_exptl_crystal_F_000             1612
_exptl_crystal_size_max          .52
_exptl_crystal_size_mid          .26
_exptl_crystal_size_min          .18
_refine_diff_density_max         1.572
_refine_diff_density_min         -3.247
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.083
_refine_ls_goodness_of_fit_obs   1.122
_refine_ls_matrix_type           full
_refine_ls_number_parameters     727
_refine_ls_number_reflns         10247
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_restrained_S_obs      1.122
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_obs          0.0429
_refine_ls_shift/esd_max         -0.541
_refine_ls_shift/esd_mean        0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0260P)^2^+20.6024P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0916
_refine_ls_wR_factor_obs         0.0827
_reflns_number_observed          8006
_reflns_number_total             10249
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            j800515sup1.cif
_cod_data_source_block           fecp1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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^)+(0.0260P)^2^+20.6024P] 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^)+(0.0260P)^2^+20.6024P] 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        2913.0(11)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7028180