Syntheses and crystallographic studies of [Ir(η5-C5Me5)(L)(RF)I] (L = CO, PMe3; RF = CF2CF3, CF2CF2CF3, CF2C6F5, CF(CF3)2) complexes. Cone and solid angle steric parameters for perfluoroalkyl ligands
Hughes, Russell P.; Smith, Jeremy M.; Liable-Sands, Louise M.; Concolino, Thomas E.; Lam, Kin-Chung; Incarvito, Christopher; Rheingold, Arnold L.; Journal of the Chemical Society, Dalton Transactions  (2000) 873–; doi:10.1039/a907057e

data_7008928
_publ_section_title
;
 Syntheses and crystallographic studies of [Ir(\h5-C5Me5)(L)(RF)I]
 (L&#x2005;=&#x2005;CO, PMe3; RF&#x2005;=&#x2005;CF2CF3, CF2CF2CF3,
 CF2C6F5, CF(CF3)2) complexes. Cone and solid angle steric parameters
 for perfluoroalkyl ligands
;
_journal_issue                   6
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              873
_journal_paper_doi               10.1039/a907057e
_journal_year                    2000
_chemical_formula_sum            'C14 H15 F7 I Ir O'
_chemical_formula_weight         651.36
_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                 94.32(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.999(9)
_cell_length_b                   14.477(5)
_cell_length_c                   13.553(7)
_cell_measurement_reflns_used    43
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      10
_cell_volume                     1761(2)
_computing_cell_refinement       Siemens/XSCANS
_computing_data_collection       Siemens/XSCANS
_computing_data_reduction        Siemens/XSCANS
_computing_molecular_graphics    XP-5.03
_computing_publication_material  XCIF
_computing_structure_refinement  'SHELXL-5.03 (Sheldrick, 1994)'
_computing_structure_solution    'SHELXS-5.03 (Sheldrick, 1994)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w 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  0.0459
_diffrn_reflns_av_sigmaI/netI    0.0682
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            3227
_diffrn_reflns_theta_max         31.62
_diffrn_reflns_theta_min         2.06
_diffrn_standards_decay_%        <7
_diffrn_standards_interval_count 197
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    9.404
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.467
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.457
_exptl_crystal_description       rod
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         3.652
_refine_diff_density_min         -1.890
_refine_diff_density_rms         0.248
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.039
_refine_ls_goodness_of_fit_obs   1.082
_refine_ls_hydrogen_treatment    'idealized contributions'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         2300
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_restrained_S_obs      1.082
_refine_ls_R_factor_all          0.1081
_refine_ls_R_factor_obs          0.0701
_refine_ls_shift/esd_max         0.045
_refine_ls_shift/esd_mean        0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0966P)^2^+41.9396P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1988
_refine_ls_wR_factor_obs         0.1692
_reflns_number_observed          1592
_reflns_number_total             2300
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            a907057e.txt
_cod_data_source_block           rph66r
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0966P)^2^+41.9396P] 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^)+(0.0966P)^2^+41.9396P] 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        1760(2)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7008928