Variable-Temperature NMR Determination of the Barriers to Rotation about the Ir-C σ-Bond in a Series of Primary Perfluoroalkyl Iridium Complexes [IrCp*{(CF2)nCF3}(PMe3)2]+X- [n =1, 2, 3, 5, 7, 9, 11; X =I, OTf]
Cheryl J. Bourgeois; Hui Huang; Roman B. Larichev; Lev N. Zakharov; Arnold L. Rheingold; Russell P. Hughes; Organometallics 26 (2007) 264–271; doi:10.1021/om060822q

data_4063253
_publ_section_title
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 Variable-Temperature NMR Determination of the Barriers to Rotation
 about the Ir-C \s-Bond in a Series of Primary Perfluoroalkyl Iridium
 Complexes [IrCp*{(CF2)nCF3}(PMe3)2]+X- [n \\db 1, 2, 3, 5, 7, 9, 11; X
 \\db I, OTf]
;
_journal_name_full               Organometallics
_journal_page_first              264
_journal_page_last               271
_journal_paper_doi               10.1021/om060822q
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C23 H24 F21 I Ir P'
_chemical_formula_weight         1049.49
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 111.080(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.772(9)
_cell_length_b                   9.545(3)
_cell_length_c                   28.600(10)
_cell_measurement_reflns_used    9899
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      28.15
_cell_measurement_theta_min      2.27
_cell_volume                     6310(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0409
_diffrn_reflns_av_sigmaI/netI    0.0402
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            34625
_diffrn_reflns_theta_full        24.00
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         1.36
_exptl_absorpt_coefficient_mu    5.401
_exptl_absorpt_correction_T_max  0.7376
_exptl_absorpt_correction_T_min  0.2941
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            dark-yellow
_exptl_crystal_density_diffrn    2.209
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3968
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.254
_refine_diff_density_min         -1.598
_refine_diff_density_rms         0.225
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         9896
_refine_ls_number_restraints     47
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0722
_refine_ls_R_factor_gt           0.0615
_refine_ls_shift/su_max          0.835
_refine_ls_shift/su_mean         0.073
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1200P)^2^+50.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1810
_refine_ls_wR_factor_ref         0.1933
_reflns_number_gt                8373
_reflns_number_total             9896
_reflns_threshold_expression     >2sigma(I)
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4063253