#------------------------------------------------------------------------------
#$Date: 2016-03-21 17:13:04 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178773 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/27/4102757.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4102757
loop_
_publ_author_name
'Christina Y. Tang'
'Amber L. Thompson'
'Simon Aldridge'
_publ_contact_author             'Simon Aldridge'
_publ_contact_author_email       simon.aldridge@chem.ox.ac.uk
_publ_section_title
;
 Dehydrogenation of Saturated CC and BN Bonds at Cationic N-Heterocyclic
 Carbene Stabilized M(III) Centers (M = Rh, Ir)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10578
_journal_page_last               10591
_journal_paper_doi               10.1021/ja1043787
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C42 H50 Cl Ir N4 Na, C32 H12 B F24'
_chemical_formula_sum            'C74 H62 B Cl F24 Ir N4 Na'
_chemical_formula_weight         1724.76
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             09-11-01
_audit_creation_method           CRYSTALS_ver_12.90
_cell_angle_alpha                90
_cell_angle_beta                 116.0509(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.7234(3)
_cell_length_b                   18.7031(3)
_cell_length_c                   19.6595(2)
_cell_measurement_reflns_used    8765
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     7506.39(18)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.038
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            60375
_diffrn_reflns_theta_full        26.921
_diffrn_reflns_theta_max         27.470
_diffrn_reflns_theta_min         5.106
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.924
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            clear_orange
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3440.002
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.040
_refine_diff_density_max         2.99
_refine_diff_density_min         -1.45
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9380
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     745
_refine_ls_number_reflns         8541
_refine_ls_number_restraints     2542
_refine_ls_R_factor_all          0.0773
_refine_ls_R_factor_gt           0.0629
_refine_ls_shift/su_max          0.0105263
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 16.8 24.5 12.0 2.97 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1556
_refine_ls_wR_factor_gt          0.1461
_refine_ls_wR_factor_ref         0.1556
_reflns_limit_h_max              26
_reflns_limit_h_min              -29
_reflns_limit_k_max              24
_reflns_limit_k_min              0
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                7236
_reflns_number_total             8541
_reflns_threshold_expression     I>2.0σ(I)
_oxford_diffrn_Wilson_B_factor   2.63
_oxford_diffrn_Wilson_scale      547.16
_oxford_refine_ls_r_factor_ref   0.0773
_oxford_refine_ls_scale          0.067693(15)
_oxford_reflns_number_all        8541
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 062ct09
_cod_data_source_file            ja1043787_si_002_03.cif
_cod_data_source_block           7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'C 1 2/c 1 '
_cod_database_code               4102757
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/2,y+1/2,z
-x+1/2,-y+1/2,-z
-x,y,-z+1/2
x,-y,z+1/2
-x+1/2,y+1/2,-z+1/2
x+1/2,-y+1/2,z+1/2
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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ir1 Ir 0.500000(9) 1.064190(17) 0.750000(9) 0.0337 1.0000 Uani S TU . . .
Cl2 Cl 0.46909(17) 1.05970(19) 0.85215(19) 0.0556 0.5000 Uani . U . 1 1
Na3 Na 0.5967(3) 1.0656(3) 0.9256(3) 0.0611 0.5000 Uani . U . 1 1
C4 C 0.5000 1.1737(4) 0.7500 0.0481 1.0000 Uani S TU . . .
N5 N 0.4457(6) 1.2147(6) 0.6942(7) 0.0462 0.5000 Uani . U . 1 2
C6 C 0.4562(8) 1.2885(7) 0.7122(8) 0.0497 0.5000 Uani . U . 1 2
C7 C 0.5090(8) 1.2927(7) 0.7775(7) 0.0512 0.5000 Uani . U . 1 1
N8 N 0.5308(6) 1.2227(6) 0.8019(8) 0.0451 0.5000 Uani . U . 1 1
C9 C 0.5859(6) 1.2074(6) 0.8736(7) 0.0397 0.5000 Uani . U . 1 1
C10 C 0.6469(8) 1.1871(8) 0.8758(9) 0.0508 0.5000 Uani . U . 1 1
C11 C 0.6962(7) 1.1722(8) 0.9470(9) 0.0603 0.5000 Uani . U . 1 1
C12 C 0.6885(8) 1.1774(10) 1.0118(12) 0.0608 0.5000 Uani . U . 1 1
C13 C 0.6275(7) 1.1979(7) 1.0078(8) 0.0540 0.5000 Uani . U . 1 1
C14 C 0.5746(7) 1.2112(6) 0.9359(8) 0.0437 0.5000 Uani . U . 1 1
C15 C 0.5086(8) 1.2324(7) 0.9328(8) 0.0565 0.5000 Uani . U . 1 1
C16 C 0.7439(9) 1.1654(9) 1.0892(10) 0.0867 0.5000 Uani . U . 1 1
C17 C 0.6580(7) 1.1855(10) 0.8072(10) 0.0707 0.5000 Uani . U . 1 1
C18 C 0.3887(10) 1.1883(7) 0.6287(7) 0.0506 0.5000 Uani . U . 1 2
C19 C 0.3334(8) 1.1640(9) 0.6384(9) 0.0577 0.5000 Uani . U . 1 2
C20 C 0.2804(8) 1.1449(9) 0.5735(9) 0.0690 0.5000 Uani . U . 1 2
C21 C 0.2764(9) 1.1503(9) 0.5014(9) 0.0741 0.5000 Uani . U . 1 2
C22 C 0.3300(10) 1.1728(12) 0.4937(11) 0.0687 0.5000 Uani . U . 1 2
C23 C 0.3887(9) 1.1920(8) 0.5589(8) 0.0567 0.5000 Uani . U . 1 2
C24 C 0.4468(10) 1.2206(9) 0.5510(8) 0.0676 0.5000 Uani . U . 1 2
C25 C 0.2128(10) 1.1295(12) 0.4328(10) 0.1105 0.5000 Uani . U . 1 2
C26 C 0.3344(7) 1.1617(10) 0.7143(8) 0.0668 0.5000 Uani . U . 1 2
C27 C 0.5000 0.9542(4) 0.7500 0.0411 1.0000 Uani S TU . . .
N28 N 0.4637(3) 0.9092(3) 0.6926(3) 0.0466 1.0000 Uani . U . . .
C29 C 0.4773(4) 0.8385(3) 0.7136(4) 0.0574 1.0000 Uani . U . . .
C30 C 0.4146(3) 0.9282(3) 0.6179(4) 0.0522 1.0000 Uani . U . . .
C31 C 0.3524(4) 0.9467(4) 0.6082(5) 0.0630 1.0000 Uani . U . . .
C32 C 0.3348(4) 0.9527(5) 0.6720(6) 0.0769 1.0000 Uani . U . . .
C33 C 0.3050(5) 0.9597(4) 0.5319(6) 0.0851 1.0000 Uani . U . . .
C34 C 0.3196(6) 0.9530(5) 0.4719(5) 0.1026 1.0000 Uani . U . . .
C35 C 0.2673(8) 0.9618(7) 0.3902(6) 0.1645 1.0000 Uani . U . . .
C36 C 0.3833(6) 0.9355(5) 0.4858(4) 0.0933 1.0000 Uani . U . . .
C37 C 0.4318(5) 0.9210(4) 0.5583(4) 0.0708 1.0000 Uani . U . . .
C38 C 0.4989(6) 0.8990(6) 0.5710(6) 0.0972 1.0000 Uani . U . . .
B39 B 0.5000 0.5663(2) 0.7500 0.0503 1.0000 Uani DS TU . . .
C40 C 0.43705(12) 0.62073(17) 0.70935(11) 0.0440 1.0000 Uani D U . . .
C41 C 0.4042(2) 0.6485(3) 0.74866(19) 0.0478 1.0000 Uani D U . . .
C42 C 0.3559(2) 0.7005(3) 0.7173(2) 0.0524 1.0000 Uani D U . . .
C43 C 0.3366(2) 0.7240(3) 0.6439(2) 0.0500 1.0000 Uani D U . . .
C44 C 0.3676(2) 0.6967(3) 0.60350(19) 0.0473 1.0000 Uani D U . . .
C45 C 0.4178(2) 0.6467(3) 0.6358(2) 0.0444 1.0000 Uani D U . . .
C46 C 0.34743(17) 0.71951(19) 0.52368(16) 0.0535 1.0000 Uani D U . . .
F47 F 0.3080(2) 0.6717(2) 0.4735(2) 0.0698 1.0000 Uani D U . . .
F48 F 0.3987(2) 0.7258(2) 0.5064(3) 0.0773 1.0000 Uani D U . . .
F49 F 0.3164(2) 0.7821(2) 0.5061(2) 0.0662 1.0000 Uani D U . . .
C50 C 0.3269(2) 0.7326(3) 0.7650(2) 0.0715 1.0000 Uani D U . . .
H111 H 0.7368 1.1580 0.9508 0.0689 0.5000 Uiso R . . 1 1
H131 H 0.6217 1.2021 1.0515 0.0609 0.5000 Uiso R . . 1 1
H151 H 0.5124 1.2363 0.9834 0.0799 0.5000 Uiso R . . 1 1
H152 H 0.4951 1.2778 0.9077 0.0799 0.5000 Uiso R . . 1 1
H153 H 0.4761 1.1968 0.9054 0.0801 0.5000 Uiso R . . 1 1
H163 H 0.7747 1.1325 1.0854 0.1240 0.5000 Uiso R . . 1 1
H162 H 0.7656 1.2097 1.1097 0.1240 0.5000 Uiso R . . 1 1
H161 H 0.7273 1.1458 1.1223 0.1239 0.5000 Uiso R . . 1 1
H171 H 0.7013 1.1678 0.8200 0.1019 0.5000 Uiso R . . 1 1
H172 H 0.6534 1.2328 0.7866 0.1020 0.5000 Uiso R . . 1 1
H173 H 0.6264 1.1544 0.7703 0.1020 0.5000 Uiso R . . 1 1
H201 H 0.2440 1.1278 0.5779 0.0851 0.5000 Uiso R . . 1 2
H221 H 0.3287 1.1747 0.4460 0.0861 0.5000 Uiso R . . 1 2
H241 H 0.4368 1.2254 0.4984 0.1061 0.5000 Uiso R . . 1 2
H242 H 0.4587 1.2665 0.5753 0.1060 0.5000 Uiso R . . 1 2
H243 H 0.4829 1.1884 0.5747 0.1060 0.5000 Uiso R . . 1 2
H253 H 0.1790 1.1633 0.4269 0.1740 0.5000 Uiso R . . 1 2
H252 H 0.1992 1.0824 0.4392 0.1740 0.5000 Uiso R . . 1 2
H251 H 0.2205 1.1304 0.3884 0.1740 0.5000 Uiso R . . 1 2
H261 H 0.3788 1.1599 0.7522 0.0991 0.5000 Uiso R . . 1 2
H262 H 0.3135 1.2035 0.7218 0.0991 0.5000 Uiso R . . 1 2
H263 H 0.3116 1.1196 0.7180 0.0990 0.5000 Uiso R . . 1 2
H291 H 0.4589 0.7983 0.6833 0.0680 1.0000 Uiso R . . . .
H323 H 0.2880 0.9520 0.6529 0.1150 1.0000 Uiso R . . . .
H322 H 0.3520 0.9973 0.6982 0.1151 1.0000 Uiso R . . . .
H321 H 0.3540 0.9128 0.7062 0.1149 1.0000 Uiso R . . . .
H331 H 0.2624 0.9735 0.5227 0.1020 1.0000 Uiso R . . . .
H353 H 0.2865 0.9845 0.3609 0.2439 1.0000 Uiso R . . . .
H352 H 0.2322 0.9907 0.3897 0.2440 1.0000 Uiso R . . . .
H351 H 0.2510 0.9156 0.3692 0.2440 1.0000 Uiso R . . . .
H361 H 0.3939 0.9330 0.4452 0.1119 1.0000 Uiso R . . . .
H381 H 0.5115 0.9243 0.5371 0.1461 1.0000 Uiso R . . . .
H382 H 0.4999 0.8486 0.5621 0.1460 1.0000 Uiso R . . . .
H383 H 0.5302 0.9091 0.6225 0.1459 1.0000 Uiso R . . . .
H411 H 0.4146 0.6313 0.7977 0.0569 1.0000 Uiso R . . . .
H451 H 0.4392 0.6300 0.6076 0.0531 1.0000 Uiso R . . . .
H431 H 0.3031 0.7579 0.6224 0.0591 1.0000 Uiso R . . . .
C540 C 0.50961(19) 0.5120(2) 0.68998(19) 0.0481 0.3154(8) Uani D U P 2 1
C550 C 0.5697(3) 0.4793(12) 0.7067(9) 0.0503 0.3154(8) Uani D U P 2 1
C560 C 0.5760(4) 0.4280(8) 0.6599(6) 0.0581 0.3154(8) Uani D U P 2 1
C570 C 0.5231(5) 0.4076(10) 0.5946(8) 0.0568 0.3154(8) Uani D U P 2 1
C580 C 0.4636(4) 0.4409(10) 0.5758(8) 0.0569 0.3154(8) Uani D U P 2 1
C590 C 0.4576(5) 0.4933(9) 0.6216(6) 0.0536 0.3154(8) Uani D U P 2 1
C600 C 0.4048(4) 0.4197(6) 0.5065(5) 0.0598 0.3154(8) Uani D U P 2 1
F610 F 0.3634(6) 0.3745(8) 0.5162(7) 0.0669 0.3154(8) Uani D U P 2 1
F620 F 0.4194(6) 0.3875(6) 0.4550(7) 0.0621 0.3154(8) Uani D U P 2 1
F630 F 0.3704(9) 0.4775(7) 0.4727(12) 0.0776 0.3154(8) Uani D U P 2 1
C640 C 0.6414(4) 0.3922(5) 0.6834(5) 0.0667 0.3154(8) Uani D U P 2 1
F650 F 0.6782(6) 0.3896(8) 0.7579(6) 0.0782 0.3154(8) Uani D U P 2 1
F660 F 0.6364(6) 0.3238(6) 0.6614(7) 0.0780 0.3154(8) Uani D U P 2 1
F670 F 0.6771(7) 0.4243(7) 0.6539(8) 0.0893 0.3154(8) Uani D U P 2 1
C541 C 0.51416(11) 0.51117(19) 0.69212(14) 0.0552 0.6846(8) Uani D U P 2 2
C551 C 0.5755(3) 0.4832(7) 0.7111(5) 0.0542 0.6846(8) Uani D U P 2 2
C561 C 0.5873(3) 0.4363(5) 0.6627(4) 0.0583 0.6846(8) Uani D U P 2 2
C571 C 0.5379(3) 0.4191(5) 0.5917(4) 0.0651 0.6846(8) Uani D U P 2 2
C581 C 0.4766(3) 0.4458(5) 0.5717(4) 0.0687 0.6846(8) Uani D U P 2 2
C591 C 0.4638(2) 0.4899(6) 0.6215(4) 0.0642 0.6846(8) Uani D U P 2 2
C601 C 0.4209(3) 0.4264(3) 0.4964(3) 0.0907 0.6846(8) Uani D U P 2 2
F611 F 0.3903(4) 0.3678(4) 0.5014(5) 0.1198 0.6846(8) Uani D U P 2 2
F621 F 0.4435(4) 0.4093(4) 0.4448(4) 0.1111 0.6846(8) Uani D U P 2 2
F631 F 0.3753(5) 0.4758(4) 0.4637(6) 0.1031 0.6846(8) Uani D U P 2 2
C641 C 0.6536(2) 0.4060(3) 0.6879(3) 0.0696 0.6846(8) Uani D U P 2 2
F651 F 0.7009(3) 0.4499(4) 0.7283(4) 0.0956 0.6846(8) Uani D U P 2 2
F661 F 0.6620(4) 0.3499(4) 0.7341(4) 0.1032 0.6846(8) Uani D U P 2 2
F671 F 0.6667(4) 0.3822(4) 0.6329(4) 0.0956 0.6846(8) Uani D U P 2 2
F510 F 0.2619(4) 0.7393(5) 0.7210(5) 0.0821 0.4411(19) Uani D U P 3 1
F520 F 0.3465(5) 0.7989(5) 0.7901(6) 0.0941 0.4411(19) Uani D U P 3 1
F530 F 0.3339(5) 0.6950(5) 0.8251(5) 0.0751 0.4411(19) Uani D U P 3 1
F511 F 0.2747(4) 0.7736(4) 0.7333(5) 0.0934 0.5589(19) Uani D U P 3 2
F521 F 0.3721(4) 0.7750(4) 0.8192(5) 0.0952 0.5589(19) Uani D U P 3 2
F531 F 0.3123(4) 0.6813(5) 0.8023(4) 0.0883 0.5589(19) Uani D U P 3 2
H5501 H 0.6065 0.4962 0.7480 0.0590 0.3154(8) Uiso R . P 2 1
H5701 H 0.5265 0.3722 0.5635 0.0630 0.3154(8) Uiso R . P 2 1
H5901 H 0.4128 0.5018 0.6169 0.0590 0.3154(8) Uiso R . P 2 1
H5511 H 0.6101 0.4958 0.7581 0.0650 0.6846(8) Uiso R . P 2 2
H5711 H 0.5466 0.3902 0.5584 0.0749 0.6846(8) Uiso R . P 2 2
H5911 H 0.4228 0.5119 0.6037 0.0710 0.6846(8) Uiso R . P 2 2
H61 H 0.4312 1.3274 0.6823 0.0614 0.5000 Uiso R . . 1 2
H71 H 0.5281 1.3355 0.8040 0.0606 0.5000 Uiso R . . 1 1
H11 H 0.5522 1.0679 0.7228 0.0510 0.5000 Uiso R . . 1 2
H12 H 0.4814 1.0649 0.6667 0.0510 0.5000 Uiso R . . 1 2
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Ir -1.4442 7.9887 27.3049 1.5928 16.7296 8.8655 15.6115 0.4179 5.8338 45.0011
11.4722 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476
0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Na 0.0362 0.0249 4.7626 3.2850 3.1736 8.8422 1.2674 0.3136 1.1128 129.4240
0.6760 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
B 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403
-0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cl2 5_656 Ir1 Cl2 . 175.99(17) yes
Cl2 5_656 Ir1 C4 . 92.00(8) yes
Cl2 . Ir1 C4 . 92.00(8) yes
Cl2 5_656 Ir1 C27 . 88.00(8) yes
Cl2 . Ir1 C27 . 88.00(8) yes
C4 . Ir1 C27 . 179.994 yes
H11 5_656 Ir1 H12 5_656 59.9 no
H11 5_656 Ir1 C4 . 87.4 no
H12 5_656 Ir1 C4 . 89.5 no
H11 5_656 Ir1 C27 . 92.6 no
H12 5_656 Ir1 C27 . 90.5 no
C4 . Ir1 C27 . 179.994 yes
H11 5_656 Ir1 H11 . 174.7 no
H12 5_656 Ir1 H11 . 120.0 no
C4 . Ir1 H11 . 87.4 no
C27 . Ir1 H11 . 92.6 no
H11 5_656 Ir1 H12 . 120.0 no
H12 5_656 Ir1 H12 . 179.0 no
C4 . Ir1 H12 . 89.5 no
C27 . Ir1 H12 . 90.5 no
H11 . Ir1 H12 . 59.9 no
Ir1 . Cl2 Na3 . 78.46(17) yes
Cl2 . Na3 C30 5_656 81.7(2) yes
Cl2 . Na3 C31 5_656 108.5(3) yes
C30 5_656 Na3 C31 5_656 29.7(2) yes
Cl2 . Na3 C14 . 83.7(4) yes
C30 5_656 Na3 C14 . 164.1(4) yes
C31 5_656 Na3 C14 . 157.5(5) yes
Ir1 . C4 N8 5_656 133.9(6) yes
Ir1 . C4 N8 . 133.9(6) yes
N8 5_656 C4 N8 . 92.1(12) yes
N5 5_656 C4 Ir1 . 121.7(6) yes
N5 5_656 C4 N5 . 116.7(11) yes
Ir1 . C4 N5 . 121.7(6) yes
C4 . N5 C6 . 109.2(10) yes
C4 . N5 C18 . 128.3(11) yes
C6 . N5 C18 . 122.5(12) yes
N5 . C6 H61 . 126.9 no
C7 5_656 C7 N8 . 106.9(9) yes
C7 5_656 C7 H71 . 118.4 no
N8 . C7 H71 . 126.1 no
C7 . N8 C4 . 113.2(11) yes
C7 . N8 C9 . 122.8(11) yes
C4 . N8 C9 . 123.7(10) yes
N8 . C9 C10 . 120.0(12) yes
N8 . C9 C14 . 116.2(13) yes
C10 . C9 C14 . 123.8(12) yes
C9 . C10 C11 . 115.5(15) yes
C9 . C10 C17 . 122.3(13) yes
C11 . C10 C17 . 122.1(16) yes
C10 . C11 C12 . 123.5(15) yes
C10 . C11 H111 . 118.2 no
C12 . C11 H111 . 118.3 no
C11 . C12 C13 . 119.6(15) yes
C11 . C12 C16 . 122.7(17) yes
C13 . C12 C16 . 117.7(19) yes
C12 . C13 C14 . 119.2(15) yes
C12 . C13 H131 . 120.6 no
C14 . C13 H131 . 120.2 no
C13 . C14 C9 . 118.3(14) yes
C13 . C14 Na3 . 78.4(8) yes
C9 . C14 Na3 . 76.8(7) yes
C13 . C14 C15 . 118.3(14) yes
C9 . C14 C15 . 123.3(12) yes
Na3 . C14 C15 . 117.0(8) yes
C14 . C15 H151 . 109.7 no
C14 . C15 H152 . 109.6 no
H151 . C15 H152 . 109.0 no
C14 . C15 H153 . 110.1 no
H151 . C15 H153 . 109.2 no
H152 . C15 H153 . 109.2 no
C12 . C16 H163 . 109.4 no
C12 . C16 H162 . 110.1 no
H163 . C16 H162 . 109.2 no
C12 . C16 H161 . 109.8 no
H163 . C16 H161 . 109.1 no
H162 . C16 H161 . 109.2 no
C10 . C17 H171 . 109.5 no
C10 . C17 H172 . 109.5 no
H171 . C17 H172 . 109.8 no
C10 . C17 H173 . 109.3 no
H171 . C17 H173 . 109.3 no
H172 . C17 H173 . 109.4 no
N5 . C18 C19 . 119.0(13) yes
N5 . C18 C23 . 118.5(17) yes
C19 . C18 C23 . 122.4(16) yes
C18 . C19 C20 . 115.3(16) yes
C18 . C19 C26 . 121.3(13) yes
C20 . C19 C26 . 123.4(17) yes
C19 . C20 C21 . 125.0(19) yes
C19 . C20 H201 . 117.5 no
C21 . C20 H201 . 117.5 no
C20 . C21 C22 . 118.6(16) yes
C20 . C21 C25 . 119.8(20) yes
C22 . C21 C25 . 121.7(18) yes
C21 . C22 C23 . 120.5(18) yes
C21 . C22 H221 . 119.6 no
C23 . C22 H221 . 119.9 no
C22 . C23 C18 . 118.2(18) yes
C22 . C23 C24 . 121.1(15) yes
C18 . C23 C24 . 120.5(15) yes
C23 . C24 H241 . 110.0 no
C23 . C24 H242 . 109.8 no
H241 . C24 H242 . 109.3 no
C23 . C24 H243 . 109.5 no
H241 . C24 H243 . 109.2 no
H242 . C24 H243 . 109.0 no
C21 . C25 H253 . 109.5 no
C21 . C25 H252 . 110.5 no
H253 . C25 H252 . 109.4 no
C21 . C25 H251 . 108.6 no
H253 . C25 H251 . 109.4 no
H252 . C25 H251 . 109.4 no
C19 . C26 H261 . 109.2 no
C19 . C26 H262 . 110.0 no
H261 . C26 H262 . 109.4 no
C19 . C26 H263 . 109.1 no
H261 . C26 H263 . 109.4 no
H262 . C26 H263 . 109.7 no
Ir1 . C27 N28 5_656 128.3(3) yes
Ir1 . C27 N28 . 128.3(3) yes
N28 5_656 C27 N28 . 103.4(7) yes
C27 . N28 C29 . 111.8(5) yes
C27 . N28 C30 . 127.4(5) yes
C29 . N28 C30 . 120.8(5) yes
N28 . C29 C29 5_656 106.5(4) yes
N28 . C29 H291 . 127.0 no
C29 5_656 C29 H291 . 126.5 no
N28 . C30 Na3 5_656 118.8(4) yes
N28 . C30 C31 . 119.1(7) yes
Na3 5_656 C30 C31 . 76.6(4) yes
N28 . C30 C37 . 117.0(7) yes
Na3 5_656 C30 C37 . 81.2(5) yes
C31 . C30 C37 . 123.7(7) yes
C30 . C31 Na3 5_656 73.8(5) yes
C30 . C31 C32 . 122.8(7) yes
Na3 5_656 C31 C32 . 116.6(5) yes
C30 . C31 C33 . 116.1(9) yes
Na3 5_656 C31 C33 . 79.1(5) yes
C32 . C31 C33 . 121.1(8) yes
C31 . C32 H323 . 109.4 no
C31 . C32 H322 . 108.7 no
H323 . C32 H322 . 109.8 no
C31 . C32 H321 . 108.8 no
H323 . C32 H321 . 110.2 no
H322 . C32 H321 . 110.0 no
C31 . C33 C34 . 122.2(10) yes
C31 . C33 H331 . 119.2 no
C34 . C33 H331 . 118.6 no
C33 . C34 C35 . 121.8(13) yes
C33 . C34 C36 . 118.7(8) yes
C35 . C34 C36 . 119.5(13) yes
C34 . C35 H353 . 109.2 no
C34 . C35 H352 . 109.2 no
H353 . C35 H352 . 109.8 no
C34 . C35 H351 . 109.3 no
H353 . C35 H351 . 109.4 no
H352 . C35 H351 . 109.9 no
C34 . C36 C37 . 122.3(10) yes
C34 . C36 H361 . 118.9 no
C37 . C36 H361 . 118.7 no
C30 . C37 C36 . 117.0(9) yes
C30 . C37 C38 . 122.0(7) yes
C36 . C37 C38 . 121.1(9) yes
C37 . C38 H381 . 110.1 no
C37 . C38 H382 . 110.1 no
H381 . C38 H382 . 108.6 no
C37 . C38 H383 . 110.4 no
H381 . C38 H383 . 109.0 no
H382 . C38 H383 . 108.6 no
C40 5_656 B39 C540 5_656 113.22(13) yes
C40 5_656 B39 C40 . 103.68(6) yes
C540 5_656 B39 C40 . 111.66(13) yes
C40 5_656 B39 C540 . 111.66(13) yes
C540 5_656 B39 C540 . 103.69(6) yes
C40 . B39 C540 . 113.22(13) yes
C541 5_656 B39 C40 5_656 115.93(8) yes
C541 5_656 B39 C40 . 109.03(8) yes
C40 5_656 B39 C40 . 103.68(6) yes
C541 5_656 B39 C541 . 103.69(6) yes
C40 5_656 B39 C541 . 109.03(8) yes
C40 . B39 C541 . 115.93(8) yes
B39 . C40 C41 . 121.66(5) yes
B39 . C40 C45 . 121.70(5) yes
C41 . C40 C45 . 116.37(5) yes
C40 . C41 C42 . 121.74(6) yes
C40 . C41 H411 . 119.1 no
C42 . C41 H411 . 119.1 no
C41 . C42 C43 . 120.83(5) yes
C41 . C42 C50 . 118.86(5) yes
C43 . C42 C50 . 120.27(5) yes
C42 . C43 C44 . 118.49(6) yes
C42 . C43 H431 . 120.5 no
C44 . C43 H431 . 121.0 no
C43 . C44 C45 . 120.80(5) yes
C43 . C44 C46 . 120.29(5) yes
C45 . C44 C46 . 118.91(5) yes
C40 . C45 C44 . 121.67(6) yes
C40 . C45 H451 . 119.3 no
C44 . C45 H451 . 119.1 no
C44 . C46 F47 . 112.4(4) yes
C44 . C46 F48 . 112.8(3) yes
F47 . C46 F48 . 104.18(9) yes
C44 . C46 F49 . 114.0(2) yes
F47 . C46 F49 . 106.75(9) yes
F48 . C46 F49 . 105.92(9) yes
C42 . C50 F510 . 107.2(5) yes
C42 . C50 F520 . 116.0(6) yes
F510 . C50 F520 . 104.15(9) yes
C42 . C50 F530 . 115.9(5) yes
F510 . C50 F530 . 106.78(9) yes
F520 . C50 F530 . 105.91(9) yes
C42 . C50 F511 . 119.4(4) yes
C42 . C50 F521 . 109.7(5) yes
F511 . C50 F521 . 104.11(9) yes
C42 . C50 F531 . 110.0(5) yes
F511 . C50 F531 . 106.81(9) yes
F521 . C50 F531 . 105.86(9) yes
B39 . C540 C550 . 121.73(6) yes
B39 . C540 C590 . 121.74(6) yes
C550 . C540 C590 . 116.44(5) yes
C540 . C550 C560 . 121.68(6) yes
C540 . C550 H5501 . 118.0 no
C560 . C550 H5501 . 120.0 no
C550 . C560 C570 . 120.76(6) yes
C550 . C560 C640 . 118.89(6) yes
C570 . C560 C640 . 120.29(6) yes
C560 . C570 C580 . 118.45(6) yes
C560 . C570 H5701 . 121.5 no
C580 . C570 H5701 . 120.1 no
C570 . C580 C590 . 120.81(5) yes
C570 . C580 C600 . 120.31(6) yes
C590 . C580 C600 . 118.88(6) yes
C540 . C590 C580 . 121.69(6) yes
C540 . C590 H5901 . 116.8 no
C580 . C590 H5901 . 116.5 no
C580 . C600 F610 . 116.4(13) yes
C580 . C600 F620 . 113.2(7) yes
F610 . C600 F620 . 104.19(9) yes
C580 . C600 F630 . 109.7(11) yes
F610 . C600 F630 . 106.78(9) yes
F620 . C600 F630 . 105.91(9) yes
C560 . C640 F650 . 114.3(7) yes
C560 . C640 F660 . 113.1(8) yes
F650 . C640 F660 . 104.11(9) yes
C560 . C640 F670 . 112.0(11) yes
F650 . C640 F670 . 106.75(9) yes
F660 . C640 F670 . 105.88(9) yes
B39 . C541 C551 . 121.72(5) yes
B39 . C541 C591 . 121.88(5) yes
C551 . C541 C591 . 116.40(5) yes
C541 . C551 C561 . 121.75(6) yes
C541 . C551 H5511 . 118.6 no
C561 . C551 H5511 . 119.7 no
C551 . C561 C571 . 120.87(5) yes
C551 . C561 C641 . 118.87(5) yes
C571 . C561 C641 . 120.26(5) yes
C561 . C571 C581 . 118.51(6) yes
C561 . C571 H5711 . 120.6 no
C581 . C571 H5711 . 120.9 no
C571 . C581 C591 . 120.75(5) yes
C571 . C581 C601 . 120.26(5) yes
C591 . C581 C601 . 118.96(5) yes
C541 . C591 C581 . 121.56(6) yes
C541 . C591 H5911 . 119.2 no
C581 . C591 H5911 . 118.4 no
C581 . C601 F611 . 111.5(7) yes
C581 . C601 F621 . 111.2(4) yes
F611 . C601 F621 . 104.06(9) yes
C581 . C601 F631 . 116.6(6) yes
F611 . C601 F631 . 106.78(9) yes
F621 . C601 F631 . 105.89(9) yes
C561 . C641 F651 . 114.1(5) yes
C561 . C641 F661 . 110.3(7) yes
F651 . C641 F661 . 104.16(9) yes
C561 . C641 F671 . 114.8(4) yes
F651 . C641 F671 . 106.77(9) yes
F661 . C641 F671 . 105.94(9) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ir1 Cl2 5_656 2.402(3) yes
Ir1 Cl2 . 2.402(3) yes
Ir1 C4 . 2.049(8) yes
Ir1 C27 . 2.058(8) yes
Ir1 H11 5_656 1.501 no
Ir1 H12 5_656 1.501 no
Ir1 C4 . 2.049(8) yes
Ir1 C27 . 2.058(8) yes
Ir1 H11 . 1.501 no
Ir1 H12 . 1.501 no
Cl2 Na3 . 2.612(7) yes
Na3 C30 5_656 2.686(9) yes
Na3 C31 5_656 2.721(10) yes
Na3 C14 . 2.792(13) yes
C4 N8 5_656 1.320(14) yes
C4 N8 . 1.320(14) yes
C4 N5 5_656 1.458(13) yes
C4 N5 . 1.458(13) yes
N5 C6 . 1.421(17) yes
N5 C18 . 1.45(2) yes
C6 C7 . 1.32(2) yes
C6 H61 . 0.950 no
C7 C7 5_656 0.97(3) yes
C7 N8 . 1.408(17) yes
C7 H71 . 0.950 no
N8 C9 . 1.446(17) yes
C9 C10 . 1.42(2) yes
C9 C14 . 1.36(2) yes
C10 C11 . 1.38(2) yes
C10 C17 . 1.48(2) yes
C11 C12 . 1.36(3) yes
C11 H111 . 0.932 no
C12 C13 . 1.41(3) yes
C12 C16 . 1.51(2) yes
C13 C14 . 1.419(19) yes
C13 H131 . 0.928 no
C14 C15 . 1.52(2) yes
C15 H151 . 0.962 no
C15 H152 . 0.962 no
C15 H153 . 0.963 no
C16 H163 . 0.958 no
C16 H162 . 0.958 no
C16 H161 . 0.958 no
C17 H171 . 0.960 no
C17 H172 . 0.960 no
C17 H173 . 0.959 no
C18 C19 . 1.43(2) yes
C18 C23 . 1.374(19) yes
C19 C20 . 1.36(2) yes
C19 C26 . 1.48(2) yes
C20 C21 . 1.38(3) yes
C20 H201 . 0.926 no
C21 C22 . 1.36(3) yes
C21 C25 . 1.53(2) yes
C22 C23 . 1.43(2) yes
C22 H221 . 0.926 no
C23 C24 . 1.49(2) yes
C24 H241 . 0.962 no
C24 H242 . 0.961 no
C24 H243 . 0.958 no
C25 H253 . 0.961 no
C25 H252 . 0.961 no
C25 H251 . 0.962 no
C26 H261 . 0.957 no
C26 H262 . 0.960 no
C26 H263 . 0.960 no
C27 N28 5_656 1.358(7) yes
C27 N28 . 1.358(7) yes
N28 C29 . 1.379(8) yes
N28 C30 . 1.446(8) yes
C29 C29 5_656 1.348(14) yes
C29 H291 . 0.936 no
C30 C31 . 1.384(11) yes
C30 C37 . 1.394(11) yes
C31 C32 . 1.479(13) yes
C31 C33 . 1.431(11) yes
C32 H323 . 0.961 no
C32 H322 . 0.967 no
C32 H321 . 0.970 no
C33 C34 . 1.366(17) yes
C33 H331 . 0.938 no
C34 C35 . 1.531(12) yes
C34 C36 . 1.388(18) yes
C35 H353 . 0.959 no
C35 H352 . 0.961 no
C35 H351 . 0.959 no
C36 C37 . 1.394(12) yes
C36 H361 . 0.931 no
C37 C38 . 1.491(14) yes
C38 H381 . 0.958 no
C38 H382 . 0.960 no
C38 H383 . 0.965 no
B39 C40 5_656 1.649(3) yes
B39 C540 5_656 1.642(4) yes
B39 C40 . 1.649(3) yes
B39 C540 . 1.642(4) yes
B39 C541 5_656 1.668(4) yes
B39 C40 5_656 1.649(3) yes
B39 C40 . 1.649(3) yes
B39 C541 . 1.668(4) yes
C40 C41 . 1.389(4) yes
C40 C45 . 1.400(4) yes
C41 C42 . 1.392(4) yes
C41 H411 . 0.943 no
C42 C43 . 1.382(4) yes
C42 C50 . 1.490(4) yes
C43 C44 . 1.371(4) yes
C43 H431 . 0.936 no
C44 C45 . 1.394(4) yes
C44 C46 . 1.491(4) yes
C45 H451 . 0.937 no
C46 F47 . 1.341(5) yes
C46 F48 . 1.353(5) yes
C46 F49 . 1.332(5) yes
C50 F510 . 1.352(7) yes
C50 F520 . 1.336(8) yes
C50 F530 . 1.322(8) yes
C50 F511 . 1.316(7) yes
C50 F521 . 1.362(7) yes
C50 F531 . 1.335(7) yes
C540 C550 . 1.396(5) yes
C540 C590 . 1.390(5) yes
C550 C560 . 1.380(5) yes
C550 H5501 . 0.929 no
C560 C570 . 1.373(5) yes
C560 C640 . 1.506(6) yes
C570 C580 . 1.383(5) yes
C570 H5701 . 0.927 no
C580 C590 . 1.377(5) yes
C580 C600 . 1.482(6) yes
C590 H5901 . 0.994 no
C600 F610 . 1.339(8) yes
C600 F620 . 1.338(8) yes
C600 F630 . 1.330(9) yes
C640 F650 . 1.331(8) yes
C640 F660 . 1.338(8) yes
C640 F670 . 1.328(9) yes
C541 C551 . 1.378(4) yes
C541 C591 . 1.414(4) yes
C551 C561 . 1.403(4) yes
C551 H5511 . 0.944 no
C561 C571 . 1.391(4) yes
C561 C641 . 1.477(5) yes
C571 C581 . 1.364(5) yes
C571 H5711 . 0.937 no
C581 C591 . 1.405(5) yes
C581 C601 . 1.510(5) yes
C591 H5911 . 0.935 no
C601 F611 . 1.326(7) yes
C601 F621 . 1.360(8) yes
C601 F631 . 1.326(7) yes
C641 F651 . 1.308(7) yes
C641 F661 . 1.346(7) yes
C641 F671 . 1.319(6) yes
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C15 . H152 C570 5_666 153 0.96 2.46 3.348(16) yes
C26 5_656 H171 C20 5_656 121 0.80 1.99 2.507(16) yes
C26 5_656 H173 N5 5_656 127 0.82 2.33 2.901(16) yes
C13 5_656 H221 C16 5_656 148 1.10 1.49 2.492(16) yes
