#------------------------------------------------------------------------------
#$Date: 2018-01-23 05:16:25 +0200 (Tue, 23 Jan 2018) $
#$Revision: 205481 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/53/7045336.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_7045336
loop_
_publ_author_name
'Congrave, Daniel G.'
'Hsu, Yu-Ting'
'Batsanov, Andrei S.'
'Beeby, Andrew'
'Bryce, Martin R.'
_publ_section_title
;
 Sky-blue emitting bridged diiridium complexes: beneficial effects of
 intramolecular π--π stacking
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C7DT04201A
_journal_year                    2018
_chemical_formula_moiety         'C58 H38 F4 Ir2 N6 O2, 3(C H2 Cl2)'
_chemical_formula_sum            'C61 H44 Cl6 F4 Ir2 N6 O2'
_chemical_formula_weight         1566.12
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-07-07
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.07.04 svn.r3439 for OlexSys, GUI svn.r5361)
;
_audit_update_record
;
2017-09-22 deposited with the CCDC.
2017-12-14 downloaded from the CCDC.
;
_cell_angle_alpha                96.8996(19)
_cell_angle_beta                 98.3065(19)
_cell_angle_gamma                113.6703(18)
_cell_formula_units_Z            1
_cell_length_a                   10.6095(6)
_cell_length_b                   11.7334(7)
_cell_length_c                   12.4455(7)
_cell_measurement_reflns_used    9956
_cell_measurement_temperature    120
_cell_measurement_theta_max      32.30
_cell_measurement_theta_min      2.43
_cell_volume                     1376.67(14)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'APEX3 v.2016.1-0 (Bruker, 2016)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2014/7 multi-CPU (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS 2013/1 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 10.4
_diffrn_detector_type            'Bruker PHOTON 100 CMOS'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       '3-circle area detector diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       ω-scan
_diffrn_radiation_monochromator  'focusing mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0526
_diffrn_reflns_av_unetI/netI     0.0371
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            73629
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        33.000
_diffrn_reflns_theta_max         34.337
_diffrn_reflns_theta_min         1.933
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\mS microsource'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.185
_exptl_absorpt_correction_T_max  0.4376
_exptl_absorpt_correction_T_min  0.3374
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
; SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) 
 was 0.1111 before and 0.0470 after correction. The Ratio of minimum to maximum 
 transmission is 0.4725. The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.889
_exptl_crystal_description       trapetsoid
_exptl_crystal_F_000             760
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.284
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.058
_refine_diff_density_max         2.051
_refine_diff_density_min         -1.310
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         11421
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0270
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0320P)²+0.6340P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0583
_refine_ls_wR_factor_ref         0.0607
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10071
_reflns_number_total             11421
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7dt04201a2.cif
_cod_data_source_block           7_16srv476
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_database_code               7045336
_shelx_shelxl_version_number     2016/6
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(Ir) = Uanis(Ir1)
3. Others
 Sof(Ir1)=1-FVAR(1)
 Sof(Ir)=FVAR(1)
 Fixed Sof: Cl3(0.5) Cl4(0.5) C31(0.5) HB(0.5) HC(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C30(H,HA), C31(HB,HC)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12),
 C14(H14), C15(H15), C16(H16), C17(H17), C20(H20), C21(H21), C22(H22), C23(H23),
  C25(H25), C27(H27), C29(H29)
;
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ir Ir 0.81434(2) 0.93517(2) 0.61721(2) 0.01242(4) Uani 0.9797(6) 1 d . P . .
F1 F 0.9411(2) 1.4002(2) 0.24673(17) 0.0469(5) Uani 1 1 d . . . .
F2 F 1.2807(2) 1.58666(15) 0.57797(18) 0.0467(5) Uani 1 1 d . . . .
O O 0.88059(17) 1.11636(15) 0.56776(14) 0.0178(3) Uani 1 1 d . . . .
N1 N 0.97058(18) 0.94193(16) 0.52007(15) 0.0148(3) Uani 1 1 d . . . .
N2 N 0.64765(19) 0.86262(17) 0.48510(16) 0.0169(3) Uani 1 1 d . . . .
N3 N 0.9683(2) 0.99853(19) 0.75665(16) 0.0189(3) Uani 1 1 d . . . .
C1 C 0.9747(2) 1.13647(19) 0.50882(17) 0.0143(3) Uani 1 1 d . . . .
C2 C 0.6659(2) 0.9511(2) 0.69208(19) 0.0178(4) Uani 1 1 d . . . .
C3 C 0.6798(3) 1.0013(2) 0.8035(2) 0.0231(4) Uani 1 1 d . . . .
H3 H 0.769775 1.037021 0.851939 0.028 Uiso 1 1 calc R . . .
C4 C 0.5627(3) 0.9995(3) 0.8443(2) 0.0284(5) Uani 1 1 d . . . .
H4 H 0.573944 1.033299 0.920151 0.034 Uiso 1 1 calc R . . .
C5 C 0.4313(3) 0.9490(3) 0.7751(2) 0.0299(5) Uani 1 1 d . . . .
H5 H 0.352244 0.946562 0.803918 0.036 Uiso 1 1 calc R . . .
C6 C 0.4141(3) 0.9018(2) 0.6635(2) 0.0257(5) Uani 1 1 d . . . .
H6 H 0.324163 0.869070 0.615415 0.031 Uiso 1 1 calc R . . .
C7 C 0.5303(2) 0.9030(2) 0.62292(19) 0.0190(4) Uani 1 1 d . . . .
C8 C 0.5229(2) 0.8566(2) 0.50647(19) 0.0181(4) Uani 1 1 d . . . .
C9 C 0.4032(2) 0.8103(2) 0.4209(2) 0.0229(5) Uani 1 1 d . . . .
H9 H 0.317123 0.808016 0.436060 0.028 Uiso 1 1 calc R . . .
C10 C 0.4102(3) 0.7680(2) 0.3143(2) 0.0261(5) Uani 1 1 d . . . .
H10 H 0.329052 0.735386 0.256028 0.031 Uiso 1 1 calc R . . .
C11 C 0.5376(3) 0.7738(2) 0.2939(2) 0.0248(5) Uani 1 1 d . . . .
H11 H 0.544877 0.744922 0.221402 0.030 Uiso 1 1 calc R . . .
C12 C 0.6535(2) 0.8222(2) 0.38041(19) 0.0204(4) Uani 1 1 d . . . .
H12 H 0.740857 0.827351 0.365770 0.024 Uiso 1 1 calc R . . .
C13 C 0.7620(2) 0.7750(2) 0.67619(19) 0.0172(4) Uani 1 1 d . . . .
C14 C 0.6454(2) 0.6570(2) 0.6333(2) 0.0209(4) Uani 1 1 d . . . .
H14 H 0.585961 0.645312 0.564095 0.025 Uiso 1 1 calc R . . .
C15 C 0.6160(3) 0.5580(2) 0.6901(2) 0.0262(5) Uani 1 1 d . . . .
H15 H 0.537331 0.479205 0.658951 0.031 Uiso 1 1 calc R . . .
C16 C 0.7002(3) 0.5724(2) 0.7923(2) 0.0282(5) Uani 1 1 d . . . .
H16 H 0.678198 0.504286 0.831121 0.034 Uiso 1 1 calc R . . .
C17 C 0.8163(3) 0.6870(2) 0.8371(2) 0.0256(5) Uani 1 1 d . . . .
H17 H 0.874372 0.697490 0.906626 0.031 Uiso 1 1 calc R . . .
C18 C 0.8475(2) 0.7868(2) 0.77963(19) 0.0200(4) Uani 1 1 d . . . .
C19 C 0.9671(2) 0.9103(2) 0.81923(19) 0.0205(4) Uani 1 1 d . . . .
C20 C 1.0768(3) 0.9423(3) 0.9109(2) 0.0273(5) Uani 1 1 d . . . .
H20 H 1.078767 0.879776 0.952277 0.033 Uiso 1 1 calc R . . .
C21 C 1.1822(3) 1.0643(3) 0.9414(2) 0.0309(6) Uani 1 1 d . . . .
H21 H 1.256741 1.086309 1.003608 0.037 Uiso 1 1 calc R . . .
C22 C 1.1777(3) 1.1544(3) 0.8800(2) 0.0289(5) Uani 1 1 d . . . .
H22 H 1.247902 1.239414 0.900709 0.035 Uiso 1 1 calc R . . .
C23 C 1.0699(3) 1.1187(2) 0.7886(2) 0.0234(4) Uani 1 1 d . . . .
H23 H 1.066983 1.180441 0.746702 0.028 Uiso 1 1 calc R . . .
C24 C 1.0261(2) 1.2613(2) 0.47323(18) 0.0161(4) Uani 1 1 d . . . .
C25 C 0.9606(2) 1.2724(2) 0.3730(2) 0.0217(4) Uani 1 1 d . . . .
H25 H 0.886564 1.200275 0.324583 0.026 Uiso 1 1 calc R . . .
C26 C 1.0054(3) 1.3905(3) 0.3449(2) 0.0281(5) Uani 1 1 d . . . .
C27 C 1.1124(3) 1.4977(2) 0.4112(3) 0.0310(6) Uani 1 1 d . . . .
H27 H 1.142022 1.577953 0.389791 0.037 Uiso 1 1 calc R . . .
C28 C 1.1746(3) 1.4828(2) 0.5102(2) 0.0287(5) Uani 1 1 d . . . .
C29 C 1.1344(3) 1.3678(2) 0.5438(2) 0.0224(4) Uani 1 1 d . . . .
H29 H 1.179235 1.361353 0.613106 0.027 Uiso 1 1 calc R . . .
Cl1 Cl 0.33532(12) 0.48012(8) 0.84406(9) 0.0577(2) Uani 1 1 d . . . .
Cl2 Cl 0.43575(12) 0.72908(9) 0.98347(7) 0.0581(3) Uani 1 1 d . . . .
C30 C 0.4037(4) 0.6435(3) 0.8493(3) 0.0430(7) Uani 1 1 d . . . .
H H 0.336407 0.662507 0.799263 0.052 Uiso 1 1 calc R . . .
HA H 0.492747 0.671339 0.822574 0.052 Uiso 1 1 calc R . . .
Cl3 Cl 0.9502(3) 1.3554(3) 0.9072(2) 0.0690(7) Uani 0.5 1 d . P A -1
Cl4 Cl 1.0961(3) 1.6131(3) 1.0387(3) 0.0964(11) Uani 0.5 1 d . P A -1
C31 C 0.9408(10) 1.4812(10) 1.0021(9) 0.064(2) Uiso 0.5 1 d . P A -1
HB H 0.866513 1.503693 0.966573 0.076 Uiso 0.5 1 calc R P A -1
HC H 0.914077 1.449761 1.069556 0.076 Uiso 0.5 1 calc R P A -1
Ir1 Ir 0.8456(7) 0.9757(8) 0.6514(6) 0.01242(4) Uani 0.0203(6) 1 d . P . .
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'
Cl Cl 0.1484 0.1585 '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'
N N 0.0061 0.0033 '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'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0.00 0.00 -1.00 0.0070
0.00 0.00 1.00 0.0290
1.00 -1.00 -1.00 0.0950
-1.00 1.00 1.00 0.0660
-1.00 -1.00 1.00 0.0420
0.00 -1.00 1.00 0.0890
0.00 1.00 0.00 0.0520
0.00 -1.00 0.00 0.0830
1.00 1.00 0.00 0.0330
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
O Ir N1 74.79(6) . .
N2 Ir O 89.01(7) . .
N2 Ir N1 95.33(7) . .
N3 Ir O 94.76(7) . .
N3 Ir N1 88.94(7) . .
N3 Ir N2 174.93(7) . .
C2 Ir O 95.99(7) . .
C2 Ir N1 169.97(7) . .
C2 Ir N2 80.34(9) . .
C2 Ir N3 95.87(9) . .
C13 Ir O 175.10(8) . .
C13 Ir N1 106.62(7) . .
C13 Ir N2 95.49(8) . .
C13 Ir N3 80.64(9) . .
C13 Ir C2 82.89(8) . .
C1 O Ir 113.50(13) . .
N1 N1 Ir 113.64(16) 2_776 .
C1 N1 Ir 133.89(14) 2_776 .
C1 N1 N1 112.5(2) 2_776 2_776
C8 N2 Ir 116.17(15) . .
C12 N2 Ir 124.83(15) . .
C12 N2 C8 119.0(2) . .
C19 N3 Ir 115.86(16) . .
C23 N3 Ir 124.58(16) . .
C23 N3 C19 119.5(2) . .
O C1 N1 125.59(19) . 2_776
O C1 C24 115.97(18) . .
N1 C1 C24 118.43(18) 2_776 .
C3 C2 Ir 128.04(18) . .
C3 C2 C7 117.1(2) . .
C7 C2 Ir 114.84(16) . .
C2 C3 C4 120.9(2) . .
C5 C4 C3 120.5(2) . .
C4 C5 C6 120.3(2) . .
C5 C6 C7 119.3(2) . .
C2 C7 C8 114.80(19) . .
C6 C7 C2 121.9(2) . .
C6 C7 C8 123.3(2) . .
N2 C8 C7 113.75(19) . .
N2 C8 C9 120.4(2) . .
C9 C8 C7 125.9(2) . .
C10 C9 C8 120.1(2) . .
C9 C10 C11 118.9(2) . .
C12 C11 C10 119.0(2) . .
N2 C12 C11 122.6(2) . .
C14 C13 Ir 128.23(17) . .
C14 C13 C18 116.9(2) . .
C18 C13 Ir 114.60(16) . .
C15 C14 C13 121.2(2) . .
C14 C15 C16 120.9(2) . .
C17 C16 C15 119.6(2) . .
C16 C17 C18 119.8(2) . .
C13 C18 C19 114.4(2) . .
C17 C18 C13 121.6(2) . .
C17 C18 C19 124.0(2) . .
N3 C19 C18 114.1(2) . .
N3 C19 C20 119.8(2) . .
C20 C19 C18 126.1(2) . .
C21 C20 C19 120.2(2) . .
C20 C21 C22 119.1(2) . .
C23 C22 C21 119.0(2) . .
N3 C23 C22 122.1(2) . .
C25 C24 C1 119.8(2) . .
C25 C24 C29 120.3(2) . .
C29 C24 C1 119.9(2) . .
C26 C25 C24 118.5(2) . .
F1 C26 C25 118.0(3) . .
F1 C26 C27 118.7(2) . .
C27 C26 C25 123.3(2) . .
C26 C27 C28 116.5(2) . .
F2 C28 C27 118.2(2) . .
F2 C28 C29 118.5(3) . .
C27 C28 C29 123.3(2) . .
C28 C29 C24 118.2(2) . .
Cl1 C30 Cl2 112.2(2) . .
Cl4 C31 Cl3 112.2(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ir O 2.1522(16) .
Ir N1 2.1708(17) .
Ir N2 2.0422(19) .
Ir N3 2.032(2) .
Ir C2 2.001(2) .
Ir C13 1.998(2) .
F1 C26 1.351(3) .
F2 C28 1.357(3) .
O C1 1.286(2) .
N1 N1 1.438(3) 2_776
N1 C1 1.312(3) 2_776
N2 C8 1.363(3) .
N2 C12 1.351(3) .
N3 C19 1.366(3) .
N3 C23 1.352(3) .
C1 C24 1.491(3) .
C2 C3 1.402(3) .
C2 C7 1.415(3) .
C3 C4 1.402(3) .
C4 C5 1.380(4) .
C5 C6 1.389(4) .
C6 C7 1.394(3) .
C7 C8 1.465(3) .
C8 C9 1.399(3) .
C9 C10 1.382(4) .
C10 C11 1.387(4) .
C11 C12 1.380(3) .
C13 C14 1.410(3) .
C13 C18 1.421(3) .
C14 C15 1.384(3) .
C15 C16 1.395(4) .
C16 C17 1.388(4) .
C17 C18 1.397(3) .
C18 C19 1.457(3) .
C19 C20 1.400(3) .
C20 C21 1.380(4) .
C21 C22 1.388(4) .
C22 C23 1.380(4) .
C24 C25 1.385(3) .
C24 C29 1.395(3) .
C25 C26 1.380(3) .
C26 C27 1.373(4) .
C27 C28 1.377(4) .
C28 C29 1.379(3) .
Cl1 C30 1.745(3) .
Cl2 C30 1.752(3) .
Cl3 C31 1.821(10) .
Cl4 C31 1.698(10) .
