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_7028179
_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            'C26 H29 Cl2 F4 Ir O P'
_chemical_formula_weight         727.56
_chemical_name_systematic
; 
 ? 
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 99.95(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.983(2)
_cell_length_b                   16.220(5)
_cell_length_c                   16.605(3)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    186(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      2.7
_cell_volume                     2648.3(11)
_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, 1996)'
_computing_publication_material  'SHELXTL/PC ver5.0 (Sheldrick, 1996)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      186(2)
_diffrn_measurement_device       'Siemens P4 diffractometer'
_diffrn_measurement_method       'omega 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  0.0427
_diffrn_reflns_av_sigmaI/netI    0.0430
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            6920
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.51
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.350
_exptl_absorpt_correction_T_max  0.498
_exptl_absorpt_correction_T_min  0.293
_exptl_absorpt_correction_type   'Blessing Acta Cryst. A, 1995, 51,33.'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.825
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1420
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.32
_refine_diff_density_max         4.399
_refine_diff_density_min         -2.595
_refine_diff_density_rms         0.283
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.025
_refine_ls_goodness_of_fit_obs   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         5466
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.163
_refine_ls_restrained_S_obs      1.010
_refine_ls_R_factor_all          0.0880
_refine_ls_R_factor_obs          0.0617
_refine_ls_shift/esd_max         0.021
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0576P)^2^+78.9000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1902
_refine_ls_wR_factor_obs         0.1450
_reflns_number_observed          4276
_reflns_number_total             5485
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            j800515sup1.cif
_cod_data_source_block           9710
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0576P)^2^+78.9000P] 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^)+(0.0576P)^2^+78.9000P] 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        2648.5(11)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7028179