data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222

_publ_contact_author_name        'Hope, Eric G.'
_publ_contact_author_email       egh1@le.ac.uk

_publ_section_title              
;
Synthesis and characterisation of some iridium-carbonyl-fluoride
complexes. Crystal structures of [IrF(CO){P(C6H4-2-CH3)3}2] and
[IrF2(COD)py2][BF4]
;
loop_
_publ_author_name
E.G.Hope
J.Fawcett
D.Harding

# Attachment '- Hope_9.cif'

data_05076
_database_code_depnum_ccdc_archive 'CCDC 720281'
#TrackingRef '- Hope_9.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C43 H42 F Ir O P2'
_chemical_formula_sum            'C43 H42 F Ir O P2'
_chemical_formula_weight         847.91

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_Int_Tables_number      14

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   10.4725(15)
_cell_length_b                   11.1807(16)
_cell_length_c                   15.201(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.106(3)
_cell_angle_gamma                90.00
_cell_volume                     1778.7(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    708
_cell_measurement_theta_min      2.69
_cell_measurement_theta_max      19.94

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             848
_exptl_absorpt_coefficient_mu    3.882
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.498
_exptl_absorpt_correction_T_max  0.733
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'

_exptl_special_details           
;
absorption correction based on 4528 reflections (SADABS); Rint 0.073
before correction and 0.033 after.
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12187
_diffrn_reflns_av_R_equivalents  0.0579
_diffrn_reflns_av_sigmaI/netI    0.0697
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.26
_diffrn_reflns_theta_max         26.00
_reflns_number_total             3499
_reflns_number_gt                2626
_reflns_threshold_expression     I>2\s(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
The Ir atom is located on a centre of symmetry and primed atoms are
generated by 1-x, 1-y, -z. The CO and F were found to be disordered,
sites of the F atom and the C of the CO group could not be resolved
and were modelled to give expected distances. The disorder is assumed
from the oxidation state of the Ir and the relative electron density of
the the C/F site with respect to the carbonyl oxygen site (\\sim 2:1)

Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0254P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3499
_refine_ls_number_parameters     229
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0470
_refine_ls_wR_factor_ref         0.0892
_refine_ls_wR_factor_gt          0.0827
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_restrained_S_all      1.083
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ir1 Ir 0.5000 0.5000 0.0000 0.03522(12) Uani 1 2 d SD . .
F1 F 0.375(2) 0.3691(16) 0.030(2) 0.041(4) Uani 0.50 1 d PD A 1
C1 C 0.407(5) 0.373(3) 0.019(4) 0.041(4) Uani 0.50 1 d PD A 2
O1 O 0.3415(9) 0.2943(9) 0.0367(6) 0.044(3) Uani 0.50 1 d PD A 2
P1 P 0.40140(15) 0.61420(16) 0.10658(10) 0.0329(4) Uani 1 1 d . A .
C2 C 0.4663(6) 0.7657(6) 0.1212(4) 0.0330(15) Uani 1 1 d . . .
C3 C 0.3926(6) 0.8649(6) 0.0991(4) 0.0366(15) Uani 1 1 d . A .
H3 H 0.3082 0.8541 0.0755 0.044 Uiso 1 1 calc R . .
C4 C 0.4399(7) 0.9793(6) 0.1108(4) 0.0454(18) Uani 1 1 d . . .
H4 H 0.3880 1.0465 0.0960 0.054 Uiso 1 1 calc R A .
C5 C 0.5625(7) 0.9952(7) 0.1440(4) 0.0531(19) Uani 1 1 d . A .
H5 H 0.5963 1.0735 0.1519 0.064 Uiso 1 1 calc R . .
C6 C 0.6357(7) 0.8975(7) 0.1657(4) 0.0487(19) Uani 1 1 d . . .
H6 H 0.7202 0.9094 0.1890 0.058 Uiso 1 1 calc R A .
C7 C 0.5908(6) 0.7827(7) 0.1548(4) 0.0424(17) Uani 1 1 d . A .
C8 C 0.6774(6) 0.6792(6) 0.1822(4) 0.0502(19) Uani 1 1 d . . .
H8A H 0.6531 0.6493 0.2399 0.075 Uiso 1 1 calc R A .
H8B H 0.7663 0.7066 0.1858 0.075 Uiso 1 1 calc R . .
H8C H 0.6686 0.6148 0.1386 0.075 Uiso 1 1 calc R . .
C9 C 0.2290(6) 0.6267(6) 0.0797(4) 0.0325(15) Uani 1 1 d . . .
C10 C 0.1431(6) 0.5811(6) 0.1389(4) 0.0356(15) Uani 1 1 d . A .
H10 H 0.1740 0.5479 0.1931 0.043 Uiso 1 1 calc R . .
C11 C 0.0132(6) 0.5837(6) 0.1195(4) 0.0399(17) Uani 1 1 d . . .
H11 H -0.0448 0.5522 0.1602 0.048 Uiso 1 1 calc R A .
C12 C -0.0320(7) 0.6319(6) 0.0413(5) 0.0494(19) Uani 1 1 d . A .
H12 H -0.1213 0.6353 0.0282 0.059 Uiso 1 1 calc R . .
C13 C 0.0523(7) 0.6751(6) -0.0176(4) 0.0469(19) Uani 1 1 d . . .
H13 H 0.0199 0.7087 -0.0713 0.056 Uiso 1 1 calc R A .
C14 C 0.1839(6) 0.6714(6) -0.0016(4) 0.0357(15) Uani 1 1 d . A .
C15 C 0.2680(7) 0.7135(7) -0.0724(4) 0.061(2) Uani 1 1 d . . .
H15A H 0.3508 0.7381 -0.0463 0.092 Uiso 1 1 calc R A .
H15B H 0.2277 0.7816 -0.1030 0.092 Uiso 1 1 calc R . .
H15C H 0.2807 0.6484 -0.1144 0.092 Uiso 1 1 calc R . .
C16 C 0.4108(6) 0.5546(6) 0.2192(4) 0.0343(15) Uani 1 1 d . . .
C17 C 0.4650(6) 0.4414(6) 0.2287(4) 0.0392(17) Uani 1 1 d . A .
H17 H 0.4896 0.3989 0.1778 0.047 Uiso 1 1 calc R . .
C18 C 0.4836(6) 0.3896(7) 0.3106(5) 0.0477(19) Uani 1 1 d . . .
H18 H 0.5194 0.3119 0.3166 0.057 Uiso 1 1 calc R A .
C19 C 0.4491(7) 0.4532(7) 0.3833(5) 0.049(2) Uani 1 1 d . A .
H19 H 0.4630 0.4195 0.4402 0.059 Uiso 1 1 calc R . .
C20 C 0.3953(6) 0.5639(7) 0.3751(4) 0.0414(17) Uani 1 1 d . . .
H20 H 0.3707 0.6049 0.4265 0.050 Uiso 1 1 calc R A .
C21 C 0.3757(5) 0.6180(6) 0.2938(4) 0.0341(15) Uani 1 1 d . A .
C22 C 0.3189(6) 0.7406(6) 0.2908(4) 0.0483(19) Uani 1 1 d . . .
H22A H 0.2707 0.7541 0.3440 0.072 Uiso 1 1 calc R A .
H22B H 0.2615 0.7480 0.2388 0.072 Uiso 1 1 calc R . .
H22C H 0.3873 0.8001 0.2879 0.072 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ir1 0.0387(2) 0.0321(2) 0.0347(2) -0.0003(2) -0.00086(14) -0.0050(2)
F1 0.046(14) 0.039(4) 0.039(9) -0.001(4) 0.017(8) -0.001(5)
C1 0.046(14) 0.039(4) 0.039(9) -0.001(4) 0.017(8) -0.001(5)
O1 0.048(6) 0.044(7) 0.040(6) -0.005(5) 0.017(4) -0.012(5)
P1 0.0365(9) 0.0316(11) 0.0303(9) 0.0015(8) -0.0030(7) 0.0009(8)
C2 0.042(4) 0.021(4) 0.036(4) -0.003(3) 0.000(3) -0.003(3)
C3 0.039(4) 0.033(4) 0.037(4) 0.001(3) 0.000(3) -0.006(3)
C4 0.064(5) 0.024(5) 0.049(4) 0.003(3) 0.007(3) 0.000(3)
C5 0.064(5) 0.040(5) 0.056(4) -0.013(4) 0.013(4) -0.023(5)
C6 0.048(4) 0.048(5) 0.051(4) -0.008(4) 0.000(3) -0.011(4)
C7 0.038(4) 0.049(5) 0.040(4) -0.003(3) -0.001(3) -0.010(4)
C8 0.041(4) 0.054(5) 0.055(5) -0.009(4) -0.016(3) -0.007(4)
C9 0.037(3) 0.028(4) 0.032(3) -0.001(3) -0.009(3) 0.002(3)
C10 0.041(4) 0.028(4) 0.037(4) -0.005(3) -0.007(3) 0.005(3)
C11 0.038(4) 0.031(4) 0.050(4) -0.006(3) -0.007(3) -0.003(3)
C12 0.043(4) 0.035(5) 0.068(5) -0.016(4) -0.021(4) 0.005(4)
C13 0.063(5) 0.034(5) 0.042(4) -0.004(3) -0.021(4) 0.008(4)
C14 0.045(4) 0.028(4) 0.034(4) 0.001(3) -0.005(3) 0.001(3)
C15 0.085(6) 0.053(6) 0.045(4) 0.017(4) -0.018(4) -0.004(4)
C16 0.027(3) 0.040(4) 0.036(4) 0.001(3) -0.005(3) 0.002(3)
C17 0.029(3) 0.042(5) 0.046(4) 0.003(3) -0.001(3) 0.002(3)
C18 0.038(4) 0.042(5) 0.062(5) 0.017(4) -0.012(3) -0.003(3)
C19 0.050(5) 0.056(5) 0.040(4) 0.014(4) -0.015(3) -0.018(4)
C20 0.040(4) 0.048(5) 0.036(4) 0.002(3) -0.004(3) -0.005(4)
C21 0.029(3) 0.038(4) 0.035(4) -0.006(3) -0.005(3) -0.001(3)
C22 0.050(4) 0.054(5) 0.040(4) -0.010(4) -0.004(3) 0.007(4)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ir1 C1 1.749(15) . ?
Ir1 C1 1.749(15) 3_665 ?
Ir1 F1 2.028(9) . ?
Ir1 F1 2.028(9) 3_665 ?
Ir1 P1 2.3334(17) 3_665 ?
Ir1 P1 2.3334(17) . ?
C1 O1 1.156(15) . ?
P1 C2 1.835(6) . ?
P1 C16 1.836(6) . ?
P1 C9 1.841(6) . ?
C2 C3 1.386(8) . ?
C2 C7 1.396(8) . ?
C3 C4 1.380(8) . ?
C3 H3 0.9500 . ?
C4 C5 1.375(9) . ?
C4 H4 0.9500 . ?
C5 C6 1.367(10) . ?
C5 H5 0.9500 . ?
C6 C7 1.376(9) . ?
C6 H6 0.9500 . ?
C7 C8 1.519(9) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.393(8) . ?
C9 C14 1.399(8) . ?
C10 C11 1.382(8) . ?
C10 H10 0.9500 . ?
C11 C12 1.372(9) . ?
C11 H11 0.9500 . ?
C12 C13 1.369(9) . ?
C12 H12 0.9500 . ?
C13 C14 1.392(9) . ?
C13 H13 0.9500 . ?
C14 C15 1.492(8) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.393(9) . ?
C16 C21 1.398(8) . ?
C17 C18 1.381(8) . ?
C17 H17 0.9500 . ?
C18 C19 1.373(9) . ?
C18 H18 0.9500 . ?
C19 C20 1.363(9) . ?
C19 H19 0.9500 . ?
C20 C21 1.385(8) . ?
C20 H20 0.9500 . ?
C21 C22 1.494(8) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Ir1 C1 180(4) . 3_665 ?
C1 Ir1 F1 8(2) . . ?
C1 Ir1 F1 172(2) 3_665 . ?
C1 Ir1 F1 172(2) . 3_665 ?
C1 Ir1 F1 8(2) 3_665 3_665 ?
F1 Ir1 F1 180.0(7) . 3_665 ?
C1 Ir1 P1 86.4(16) . 3_665 ?
C1 Ir1 P1 93.6(17) 3_665 3_665 ?
F1 Ir1 P1 93.9(6) . 3_665 ?
F1 Ir1 P1 86.1(6) 3_665 3_665 ?
C1 Ir1 P1 93.6(16) . . ?
C1 Ir1 P1 86.4(17) 3_665 . ?
F1 Ir1 P1 86.1(6) . . ?
F1 Ir1 P1 93.9(6) 3_665 . ?
P1 Ir1 P1 180.0 3_665 . ?
O1 C1 Ir1 175(4) . . ?
C2 P1 C16 102.4(3) . . ?
C2 P1 C9 108.2(3) . . ?
C16 P1 C9 104.7(3) . . ?
C2 P1 Ir1 114.7(2) . . ?
C16 P1 Ir1 116.0(2) . . ?
C9 P1 Ir1 110.02(19) . . ?
C3 C2 C7 118.9(6) . . ?
C3 C2 P1 120.6(5) . . ?
C7 C2 P1 120.4(5) . . ?
C4 C3 C2 121.1(6) . . ?
C4 C3 H3 119.4 . . ?
C2 C3 H3 119.4 . . ?
C5 C4 C3 119.5(7) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
C6 C5 C4 119.5(7) . . ?
C6 C5 H5 120.2 . . ?
C4 C5 H5 120.2 . . ?
C5 C6 C7 122.0(7) . . ?
C5 C6 H6 119.0 . . ?
C7 C6 H6 119.0 . . ?
C6 C7 C2 118.8(7) . . ?
C6 C7 C8 118.7(6) . . ?
C2 C7 C8 122.5(6) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 C14 119.7(6) . . ?
C10 C9 P1 118.7(4) . . ?
C14 C9 P1 121.3(5) . . ?
C11 C10 C9 120.6(6) . . ?
C11 C10 H10 119.7 . . ?
C9 C10 H10 119.7 . . ?
C12 C11 C10 119.9(6) . . ?
C12 C11 H11 120.0 . . ?
C10 C11 H11 120.0 . . ?
C13 C12 C11 119.7(6) . . ?
C13 C12 H12 120.1 . . ?
C11 C12 H12 120.1 . . ?
C12 C13 C14 122.2(6) . . ?
C12 C13 H13 118.9 . . ?
C14 C13 H13 118.9 . . ?
C13 C14 C9 117.8(6) . . ?
C13 C14 C15 118.1(6) . . ?
C9 C14 C15 124.1(6) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 C21 119.7(6) . . ?
C17 C16 P1 115.7(5) . . ?
C21 C16 P1 124.4(5) . . ?
C18 C17 C16 121.1(7) . . ?
C18 C17 H17 119.4 . . ?
C16 C17 H17 119.4 . . ?
C19 C18 C17 118.5(7) . . ?
C19 C18 H18 120.8 . . ?
C17 C18 H18 120.8 . . ?
C20 C19 C18 121.1(7) . . ?
C20 C19 H19 119.5 . . ?
C18 C19 H19 119.5 . . ?
C19 C20 C21 121.7(7) . . ?
C19 C20 H20 119.1 . . ?
C21 C20 H20 119.1 . . ?
C20 C21 C16 117.8(6) . . ?
C20 C21 C22 118.3(6) . . ?
C16 C21 C22 123.9(6) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 Ir1 P1 C2 178(3) . . . . ?
C1 Ir1 P1 C2 -2(3) 3_665 . . . ?
F1 Ir1 P1 C2 -179.4(10) . . . . ?
F1 Ir1 P1 C2 0.6(10) 3_665 . . . ?
C1 Ir1 P1 C16 59(3) . . . . ?
C1 Ir1 P1 C16 -121(3) 3_665 . . . ?
F1 Ir1 P1 C16 61.4(10) . . . . ?
F1 Ir1 P1 C16 -118.6(10) 3_665 . . . ?
C1 Ir1 P1 C9 -60(3) . . . . ?
C1 Ir1 P1 C9 120(3) 3_665 . . . ?
F1 Ir1 P1 C9 -57.1(10) . . . . ?
F1 Ir1 P1 C9 122.9(10) 3_665 . . . ?
C16 P1 C2 C3 -119.8(5) . . . . ?
C9 P1 C2 C3 -9.6(6) . . . . ?
Ir1 P1 C2 C3 113.6(5) . . . . ?
C16 P1 C2 C7 60.3(5) . . . . ?
C9 P1 C2 C7 170.5(5) . . . . ?
Ir1 P1 C2 C7 -66.3(5) . . . . ?
C7 C2 C3 C4 -0.8(9) . . . . ?
P1 C2 C3 C4 179.3(5) . . . . ?
C2 C3 C4 C5 0.7(10) . . . . ?
C3 C4 C5 C6 -0.5(10) . . . . ?
C4 C5 C6 C7 0.4(10) . . . . ?
C5 C6 C7 C2 -0.5(10) . . . . ?
C5 C6 C7 C8 -178.8(6) . . . . ?
C3 C2 C7 C6 0.7(9) . . . . ?
P1 C2 C7 C6 -179.4(5) . . . . ?
C3 C2 C7 C8 178.9(6) . . . . ?
P1 C2 C7 C8 -1.1(8) . . . . ?
C2 P1 C9 C10 -115.2(5) . . . . ?
C16 P1 C9 C10 -6.5(6) . . . . ?
Ir1 P1 C9 C10 118.8(5) . . . . ?
C2 P1 C9 C14 70.3(6) . . . . ?
C16 P1 C9 C14 179.0(5) . . . . ?
Ir1 P1 C9 C14 -55.7(6) . . . . ?
C14 C9 C10 C11 -2.5(9) . . . . ?
P1 C9 C10 C11 -177.1(5) . . . . ?
C9 C10 C11 C12 -0.2(10) . . . . ?
C10 C11 C12 C13 1.2(10) . . . . ?
C11 C12 C13 C14 0.4(10) . . . . ?
C12 C13 C14 C9 -3.0(10) . . . . ?
C12 C13 C14 C15 176.1(6) . . . . ?
C10 C9 C14 C13 4.0(9) . . . . ?
P1 C9 C14 C13 178.4(5) . . . . ?
C10 C9 C14 C15 -175.1(6) . . . . ?
P1 C9 C14 C15 -0.7(9) . . . . ?
C2 P1 C16 C17 -131.7(5) . . . . ?
C9 P1 C16 C17 115.4(5) . . . . ?
Ir1 P1 C16 C17 -6.0(5) . . . . ?
C2 P1 C16 C21 43.9(6) . . . . ?
C9 P1 C16 C21 -69.0(6) . . . . ?
Ir1 P1 C16 C21 169.6(4) . . . . ?
C21 C16 C17 C18 0.7(9) . . . . ?
P1 C16 C17 C18 176.5(5) . . . . ?
C16 C17 C18 C19 -1.0(9) . . . . ?
C17 C18 C19 C20 1.3(10) . . . . ?
C18 C19 C20 C21 -1.5(10) . . . . ?
C19 C20 C21 C16 1.1(9) . . . . ?
C19 C20 C21 C22 -178.6(6) . . . . ?
C17 C16 C21 C20 -0.8(9) . . . . ?
P1 C16 C21 C20 -176.2(5) . . . . ?
C17 C16 C21 C22 179.0(6) . . . . ?
P1 C16 C21 C22 3.6(9) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.197
_refine_diff_density_min         -0.739
_refine_diff_density_rms         0.113

# Attachment '- Hope_15.cif'

data_04213
_database_code_depnum_ccdc_archive 'CCDC 720282'
#TrackingRef '- Hope_15.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H22 F2 Ir N2, B F4'
_chemical_formula_sum            'C18 H22 B F6 Ir N2'
_chemical_formula_weight         583.39

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'I 41/a c d'
_symmetry_space_group_name_Hall  '-I 4bd 2c'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+1/4, x+3/4, z+1/4'
'y+1/4, -x+1/4, z+3/4'
'-x+1/2, y, -z'
'x, -y, -z+1/2'
'y+1/4, x+3/4, -z+3/4'
'-y+1/4, -x+1/4, -z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+3/4, x+5/4, z+3/4'
'y+3/4, -x+3/4, z+5/4'
'-x+1, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1'
'y+3/4, x+5/4, -z+5/4'
'-y+3/4, -x+3/4, -z+3/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-1/4, -x-3/4, -z-1/4'
'-y-1/4, x-1/4, -z-3/4'
'x-1/2, -y, z'
'-x, y, z-1/2'
'-y-1/4, -x-3/4, z-3/4'
'y-1/4, x-1/4, z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y+1/4, -x-1/4, -z+1/4'
'-y+1/4, x+1/4, -z-1/4'
'x, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z'
'-y+1/4, -x-1/4, z-1/4'
'y+1/4, x+1/4, z+1/4'

_cell_length_a                   17.4108(15)
_cell_length_b                   17.4108(15)
_cell_length_c                   25.463(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     7718.8(13)
_cell_formula_units_Z            16
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    2598
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      23.00

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.008
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4480
_exptl_absorpt_coefficient_mu    6.981
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.413
_exptl_absorpt_correction_T_max  0.811
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'

_exptl_special_details           
;
absorption correction based on 5199 reflections (SADABS); Rint 0.080 before
correction and 0.054 after.
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            23152
_diffrn_reflns_av_R_equivalents  0.1342
_diffrn_reflns_av_sigmaI/netI    0.0632
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         2.30
_diffrn_reflns_theta_max         26.00
_reflns_number_total             1904
_reflns_number_gt                1333
_reflns_threshold_expression     I>2\s(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0700P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1904
_refine_ls_number_parameters     125
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0879
_refine_ls_R_factor_gt           0.0553
_refine_ls_wR_factor_ref         0.1353
_refine_ls_wR_factor_gt          0.1223
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.027
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ir1 Ir 0.2500 0.38172(3) 0.0000 0.0317(2) Uani 1 2 d S . .
F1 F 0.2580(3) 0.3948(3) 0.0780(2) 0.0389(14) Uani 1 1 d . . .
N1 N 0.1649(5) 0.4690(5) 0.0036(4) 0.0369(19) Uani 1 1 d . . .
C1 C 0.1652(6) 0.2954(7) 0.0302(5) 0.043(3) Uani 1 1 d . . .
H1 H 0.1348 0.3361 0.0438 0.051 Uiso 1 1 calc R . .
C2 C 0.2041(8) 0.2448(7) 0.0693(5) 0.050(3) Uani 1 1 d . . .
H2A H 0.1740 0.1969 0.0733 0.060 Uiso 1 1 calc R . .
H2B H 0.2051 0.2710 0.1038 0.060 Uiso 1 1 calc R . .
C3 C 0.2892(8) 0.2237(7) 0.0527(5) 0.055(3) Uani 1 1 d . . .
H3A H 0.3185 0.2091 0.0844 0.066 Uiso 1 1 calc R . .
H3B H 0.2878 0.1785 0.0291 0.066 Uiso 1 1 calc R . .
C4 C 0.3306(7) 0.2887(7) 0.0252(5) 0.049(3) Uani 1 1 d . . .
H4 H 0.3549 0.3268 0.0460 0.059 Uiso 1 1 calc R . .
C5 C 0.1381(6) 0.5007(8) -0.0409(5) 0.049(3) Uani 1 1 d . . .
H5 H 0.1555 0.4823 -0.0739 0.059 Uiso 1 1 calc R . .
C6 C 0.0866(6) 0.5585(7) -0.0390(5) 0.048(3) Uani 1 1 d . . .
H6 H 0.0666 0.5784 -0.0710 0.058 Uiso 1 1 calc R . .
C7 C 0.0617(6) 0.5900(7) 0.0081(5) 0.047(3) Uani 1 1 d . . .
H7 H 0.0272 0.6322 0.0094 0.056 Uiso 1 1 calc R . .
C8 C 0.0906(6) 0.5556(7) 0.0530(5) 0.045(3) Uani 1 1 d . . .
H8 H 0.0751 0.5735 0.0866 0.054 Uiso 1 1 calc R . .
C9 C 0.1423(6) 0.4948(7) 0.0491(5) 0.043(3) Uani 1 1 d . . .
H9 H 0.1614 0.4716 0.0802 0.052 Uiso 1 1 calc R . .
F2 F 0.9793(6) 0.6879(7) 0.0977(5) 0.181(7) Uani 1 1 d . . .
B1 B 1.0000 0.7500 0.1250 0.028(6) Uani 1 4 d S . .
F3 F 0.9978(7) 0.3109(6) 0.0963(5) 0.148(5) Uani 1 1 d . . .
B2 B 1.0000 0.2500 0.1250 0.148(5) Uani 1 4 d S . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ir1 0.0306(3) 0.0378(3) 0.0268(3) 0.000 -0.0007(3) 0.000
F1 0.039(3) 0.051(3) 0.027(3) 0.004(2) 0.004(3) 0.008(3)
N1 0.038(5) 0.047(5) 0.026(5) 0.003(4) 0.001(4) -0.004(4)
C1 0.038(6) 0.042(7) 0.048(8) 0.003(6) 0.003(6) -0.004(5)
C2 0.067(9) 0.050(8) 0.032(7) 0.010(5) 0.007(7) -0.011(6)
C3 0.078(9) 0.048(8) 0.040(7) -0.005(6) 0.001(6) 0.018(7)
C4 0.048(7) 0.051(8) 0.049(8) 0.002(6) -0.010(6) 0.020(6)
C5 0.049(6) 0.064(8) 0.034(7) 0.007(7) -0.005(5) 0.014(8)
C6 0.046(7) 0.061(8) 0.038(7) 0.014(6) -0.009(5) 0.003(6)
C7 0.032(6) 0.044(6) 0.065(9) 0.001(6) 0.003(6) -0.003(5)
C8 0.040(6) 0.046(7) 0.048(8) -0.004(6) 0.008(5) -0.001(5)
C9 0.046(6) 0.046(6) 0.038(7) 0.018(6) 0.001(5) -0.007(7)
F2 0.125(9) 0.211(12) 0.207(13) -0.166(10) -0.111(9) 0.094(9)
B1 0.023(8) 0.023(8) 0.039(16) 0.000 0.000 0.000
F3 0.161(11) 0.098(8) 0.185(13) 0.073(8) 0.014(9) 0.057(7)
B2 0.161(11) 0.098(8) 0.185(13) 0.073(8) 0.014(9) 0.057(7)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ir1 F1 2.003(6) . ?
Ir1 N1 2.124(9) . ?
Ir1 C4 2.237(11) . ?
Ir1 C1 2.242(11) . ?
N1 C9 1.303(14) . ?
N1 C5 1.344(14) . ?
C1 C2 1.491(15) . ?
C1 H1 0.9500 . ?
C2 C3 1.584(16) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.514(15) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4 0.9500 . ?
C5 C6 1.349(15) . ?
C5 H5 0.9500 . ?
C6 C7 1.387(16) . ?
C6 H6 0.9500 . ?
C7 C8 1.387(16) . ?
C7 H7 0.9500 . ?
C8 C9 1.393(15) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
F2 B1 1.334(10) . ?
F3 B2 1.287(9) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
F1 Ir1 F1 167.0(3) . 5 ?
F1 Ir1 N1 85.7(3) . . ?
F1 Ir1 N1 85.0(3) 5 . ?
N1 Ir1 N1 88.6(4) . 5 ?
F1 Ir1 C4 114.2(4) . 5 ?
F1 Ir1 C4 75.8(4) 5 5 ?
N1 Ir1 C4 95.3(4) . 5 ?
N1 Ir1 C4 160.6(4) 5 5 ?
F1 Ir1 C4 75.8(4) . . ?
F1 Ir1 C4 114.2(4) 5 . ?
N1 Ir1 C4 160.6(4) . . ?
N1 Ir1 C4 95.3(4) 5 . ?
C4 Ir1 C4 87.2(7) 5 . ?
F1 Ir1 C1 77.4(4) . . ?
F1 Ir1 C1 111.8(3) 5 . ?
N1 Ir1 C1 90.3(4) . . ?
N1 Ir1 C1 162.4(4) 5 . ?
C4 Ir1 C1 36.9(4) 5 . ?
C4 Ir1 C1 80.2(4) . . ?
F1 Ir1 C1 111.8(3) . 5 ?
F1 Ir1 C1 77.4(4) 5 5 ?
N1 Ir1 C1 162.4(4) . 5 ?
N1 Ir1 C1 90.3(4) 5 5 ?
C4 Ir1 C1 80.2(4) 5 5 ?
C4 Ir1 C1 36.9(4) . 5 ?
C1 Ir1 C1 95.9(6) . 5 ?
C9 N1 C5 120.2(10) . . ?
C9 N1 Ir1 119.7(8) . . ?
C5 N1 Ir1 120.0(8) . . ?
C4 C1 C2 126.2(12) 5 . ?
C4 C1 Ir1 71.4(7) 5 . ?
C2 C1 Ir1 109.1(8) . . ?
C4 C1 H1 116.9 5 . ?
C2 C1 H1 116.9 . . ?
Ir1 C1 H1 89.6 . . ?
C1 C2 C3 112.6(10) . . ?
C1 C2 H2A 109.1 . . ?
C3 C2 H2A 109.1 . . ?
C1 C2 H2B 109.1 . . ?
C3 C2 H2B 109.1 . . ?
H2A C2 H2B 107.8 . . ?
C4 C3 C2 113.3(10) . . ?
C4 C3 H3A 108.9 . . ?
C2 C3 H3A 108.9 . . ?
C4 C3 H3B 108.9 . . ?
C2 C3 H3B 108.9 . . ?
H3A C3 H3B 107.7 . . ?
C1 C4 C3 123.1(11) 5 . ?
C1 C4 Ir1 71.8(7) 5 . ?
C3 C4 Ir1 112.0(8) . . ?
C1 C4 H4 118.4 5 . ?
C3 C4 H4 118.4 . . ?
Ir1 C4 H4 86.2 . . ?
N1 C5 C6 120.5(12) . . ?
N1 C5 H5 119.7 . . ?
C6 C5 H5 119.7 . . ?
C5 C6 C7 122.2(11) . . ?
C5 C6 H6 118.9 . . ?
C7 C6 H6 118.9 . . ?
C6 C7 C8 115.4(11) . . ?
C6 C7 H7 122.3 . . ?
C8 C7 H7 122.3 . . ?
C7 C8 C9 120.2(11) . . ?
C7 C8 H8 119.9 . . ?
C9 C8 H8 119.9 . . ?
N1 C9 C8 121.4(11) . . ?
N1 C9 H9 119.3 . . ?
C8 C9 H9 119.3 . . ?
F2 B1 F2 105.7(7) 27_575 . ?
F2 B1 F2 117.3(14) . 10_664 ?
F3 B2 F3 105.8(10) 8_665 . ?
F3 B2 F3 111.8(12) . 15_534 ?
F3 B2 F3 110.9(13) . 10_654 ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.887
_refine_diff_density_min         -2.214
_refine_diff_density_rms         0.204