Synthesis, structure, and reactivity of iridium perfluorocarbene complexes: regio- and stereo-specific addition of HCl across a metal carbon double bond.
Yuan, Jian; Bourgeois, Cheryl J.; Rheingold, Arnold L.; Hughes, Russell P.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 19528–19542; doi:10.1039/c5dt02275d

data_7035904
_publ_section_title
;
 Synthesis, structure, and reactivity of iridium perfluorocarbene
 complexes: regio- and stereo-specific addition of HCl across a metal
 carbon double bond.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              19528
_journal_page_last               19542
_journal_paper_doi               10.1039/c5dt02275d
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C16 H24 F6 Ir P'
_chemical_formula_sum            'C16 H24 F6 Ir P'
_chemical_formula_weight         553.52
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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
_audit_creation_date             2015-07-13
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-07-14 deposited with the CCDC.
2015-07-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.450(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.379(5)
_cell_length_b                   13.834(7)
_cell_length_c                   17.073(9)
_cell_measurement_reflns_used    9411
_cell_measurement_temperature    218.15
_cell_measurement_theta_max      27.875
_cell_measurement_theta_min      2.426
_cell_volume                     1946.2(18)
_computing_cell_refinement       'SAINT v7.06A (Bruker, 2003)'
_computing_data_reduction        'SAINT v7.06A (Bruker, 2003)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      218.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.908
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_av_unetI/netI     0.0340
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.908
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            13762
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.908
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.134
_diffrn_reflns_theta_min         2.426
_exptl_absorpt_coefficient_mu    6.992
_exptl_absorpt_correction_T_max  0.6552
_exptl_absorpt_correction_T_min  0.525861
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.1324 before and 0.0385 after correction.
The Ratio of minimum to maximum transmission is 0.5259.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            YELLOW
_exptl_crystal_density_diffrn    1.889
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.802
_refine_diff_density_min         -1.561
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         4323
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0320
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0375P)^2^+4.5862P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0796
_refine_ls_wR_factor_ref         0.0829
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3812
_reflns_number_total             4323
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt02275d2.cif
_cod_data_source_block           rph342
_cod_depositor_comments
'Adding full bibliography for 7035903--7035909.cif.'
_cod_database_code               7035904
_shelx_estimated_absorpt_t_max   0.542
_shelx_estimated_absorpt_t_min   0.193
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C12-F2 = C12-F2A = C12-F3 = C12-F3A
 1.4 with sigma of 0.02
 C13-F4 = C13-F4A = C13-F5 = C13-F5A = C13-F6 = C13-F6A
 1.35 with sigma of 0.02
3. Others
 Sof(F2A)=Sof(F3A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=1-FVAR(1)
 Sof(F2)=Sof(F3)=Sof(F4)=Sof(F5)=Sof(F6)=FVAR(1)
4.a Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,
 H10B,H10C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              99858
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'