Synthesis and Structural and Computational Studies of a Conformationally Locked (η1-Perfluoroalkylidene)(η2-alkene) Transition Metal Complex: Ir(Cp*)(CFCF3)(C2H4)
Yuan, Jian; Hughes, Russell P.; Golen, James A.; Rheingold, Arnold L.; Organometallics 29 (2010) 1942–; doi:10.1021/om1000343

data_4065617
_publ_section_title
;
 Synthesis and Structural and Computational Studies of a Conformationally
 Locked (\h1-Perfluoroalkylidene)(\h2-alkene) Transition Metal Complex:
 Ir(Cp*)(CFCF3)(C2H4)
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              1942
_journal_paper_doi               10.1021/om1000343
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C24 H30 F10 I2 Ir2'
_chemical_formula_weight         1146.68
_chemical_name_systematic
; 
 ? 
;
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.8514(10)
_cell_length_b                   13.9753(11)
_cell_length_c                   16.3838(13)
_cell_measurement_reflns_used    9993
_cell_measurement_temperature    208(2)
_cell_measurement_theta_max      28.05
_cell_measurement_theta_min      2.49
_cell_volume                     2942.6(4)
_computing_cell_refinement       'Bruker APEX II SMART'
_computing_data_collection       'Bruker AEPX II SMART'
_computing_data_reduction        'Bruker APEX II 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      208(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.976
_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  0.0447
_diffrn_reflns_av_sigmaI/netI    0.0233
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            35687
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.08
_diffrn_reflns_theta_min         2.49
_exptl_absorpt_coefficient_mu    11.211
_exptl_absorpt_correction_T_max  0.5678
_exptl_absorpt_correction_T_min  0.5678
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.588
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             2096
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.070
_refine_diff_density_min         -0.840
_refine_diff_density_rms         0.150
_refine_ls_extinction_coef       0.00042(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         3497
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0217
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0288P)^2^+4.1832P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0501
_refine_ls_wR_factor_ref         0.0545
_reflns_number_gt                2874
_reflns_number_total             3497
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om1000343_si_002.cif
_cod_data_source_block           rph427_COMPOUND_11
_cod_depositor_comments
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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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               4065617