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#$Date: 2019-11-25 15:42:14 +0200 (Mon, 25 Nov 2019) $
#$Revision: 241234 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/08/4130876.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_4130876
loop_
_publ_author_name
'Sharninghausen, Liam S.'
'Sinha, Shashi Bhushan'
'Shopov, Dimitar Y.'
'Choi, Bonnie'
'Mercado, Brandon Q.'
'Roy, Xavier'
'Balcells, David'
'Brudvig, Gary W.'
'Crabtree, Robert H.'
_publ_section_title
;
 High Oxidation State Iridium Mono-μ-oxo Dimers Related to Water
 Oxidation Catalysis.
;
_journal_issue                   49
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15917
_journal_page_last               15926
_journal_paper_doi               10.1021/jacs.6b07716
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C32 H40 Cl2 Ir2 N4 O5'
_chemical_formula_sum            'C32 H40 Cl2 Ir2 N4 O5'
_chemical_formula_weight         1015.98
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 98.991(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.2543(15)
_cell_length_b                   8.3385(6)
_cell_length_c                   18.2152(12)
_cell_measurement_reflns_used    6372
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      67.0950
_cell_measurement_theta_min      3.9500
_cell_volume                     3338.6(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41o (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41o (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41o (Rigaku OD, 2015)'
_computing_molecular_graphics
; 
Dolomanov, O.V.; Bourhis, L.J.; Gildea, R.J.; Howard, J.A.K.; Puschmann, H., 
OLEX2: A complete structure solution, refinement and analysis program 
(2009). J. Appl. Cryst., 42, 339-341. 
;
_computing_publication_material  'SHELXL-2013/2 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 22.2
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1533
_diffrn_reflns_av_unetI/netI     0.0704
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            27605
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.907
_diffrn_reflns_theta_min         4.022
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    17.060
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69398
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.38.41o (Rigaku Oxford Diffraction, 2015) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.021
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         3.317
_refine_diff_density_min         -3.487
_refine_diff_density_rms         0.427
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.180
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         2956
_refine_ls_number_restraints     225
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.1204
_refine_ls_R_factor_gt           0.0874
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1090P)²+414.9259P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2241
_refine_ls_wR_factor_ref         0.2620
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2261
_reflns_number_total             2956
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja6b07716_si_002.cif
_cod_data_source_block           007-16008-2
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4130876
_shelx_shelxl_version_number     2014/7
_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. 
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'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_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Ir1 Ir 0.41462(4) 0.60459(11) 0.23408(5) 0.0263(4) Uani 1 1 d . U .
Cl02 Cl 0.4240(3) 0.4549(7) 0.1262(3) 0.0373(13) Uani 1 1 d . U .
O1 O 0.4052(7) 0.7321(19) 0.3211(8) 0.033(3) Uani 1 1 d . U .
O2 O 0.3273(7) 0.572(2) 0.2144(9) 0.037(3) Uani 1 1 d . U .
O3 O 0.5000 0.652(3) 0.2500 0.035(4) Uani 1 2 d S TU P
N1 N 0.4211(8) 0.419(2) 0.3084(9) 0.025(3) Uani 1 1 d . U .
N2 N 0.3949(9) 0.800(2) 0.1678(10) 0.031(3) Uani 1 1 d . U .
C1 C 0.4226(11) 0.257(3) 0.2887(15) 0.035(4) Uani 1 1 d . U .
H1 H 0.4259 0.2282 0.2402 0.042 Uiso 1 1 calc R U .
C2 C 0.4192(12) 0.145(3) 0.3401(15) 0.041(5) Uani 1 1 d . U .
H2 H 0.4220 0.0377 0.3272 0.049 Uiso 1 1 calc R U .
C3 C 0.4114(10) 0.184(3) 0.4128(14) 0.035(4) Uani 1 1 d . U .
H3 H 0.4092 0.1059 0.4488 0.043 Uiso 1 1 calc R U .
C4 C 0.4071(10) 0.349(3) 0.4274(13) 0.031(4) Uani 1 1 d . U .
H4 H 0.4012 0.3813 0.4747 0.037 Uiso 1 1 calc R U .
C5 C 0.4112(10) 0.463(3) 0.3749(12) 0.027(4) Uani 1 1 d . U .
C6 C 0.4576(10) 0.697(3) 0.4484(11) 0.030(4) Uani 1 1 d . U .
H6A H 0.4953 0.6731 0.4315 0.045 Uiso 1 1 calc R U .
H6B H 0.4559 0.6417 0.4942 0.045 Uiso 1 1 calc R U .
H6C H 0.4549 0.8106 0.4563 0.045 Uiso 1 1 calc R U .
C7 C 0.4033(11) 0.642(3) 0.3884(13) 0.032(3) Uani 1 1 d . U .
C8 C 0.3423(11) 0.675(3) 0.4136(13) 0.036(4) Uani 1 1 d . U .
H8A H 0.3385 0.7879 0.4224 0.054 Uiso 1 1 calc R U .
H8B H 0.3401 0.6172 0.4586 0.054 Uiso 1 1 calc R U .
H8C H 0.3100 0.6412 0.3757 0.054 Uiso 1 1 calc R U .
C9 C 0.4379(12) 0.907(3) 0.1504(12) 0.035(4) Uani 1 1 d . U .
H9 H 0.4791 0.8887 0.1663 0.042 Uiso 1 1 calc R U .
C10 C 0.4182(12) 1.041(3) 0.1085(12) 0.035(4) Uani 1 1 d . U .
H10 H 0.4463 1.1129 0.0944 0.042 Uiso 1 1 calc R U .
C11 C 0.3584(12) 1.067(3) 0.0886(12) 0.039(5) Uani 1 1 d . U .
H11 H 0.3458 1.1589 0.0613 0.046 Uiso 1 1 calc R U .
C12 C 0.3136(12) 0.960(3) 0.1077(12) 0.035(4) Uani 1 1 d . U .
H12 H 0.2722 0.9796 0.0945 0.043 Uiso 1 1 calc R U .
C13 C 0.3360(11) 0.821(3) 0.1481(13) 0.037(4) Uani 1 1 d . U .
C14 C 0.2498(11) 0.770(3) 0.2177(12) 0.036(5) Uani 1 1 d . U .
H14A H 0.2272 0.6865 0.2370 0.054 Uiso 1 1 calc R U .
H14B H 0.2222 0.8418 0.1879 0.054 Uiso 1 1 calc R U .
H14C H 0.2725 0.8290 0.2583 0.054 Uiso 1 1 calc R U .
C15 C 0.2929(11) 0.699(3) 0.1709(13) 0.036(4) Uani 1 1 d . U .
C16 C 0.2562(13) 0.615(3) 0.1013(15) 0.047(5) Uani 1 1 d . U .
H16A H 0.2839 0.5754 0.0701 0.071 Uiso 1 1 calc R U .
H16B H 0.2289 0.6909 0.0740 0.071 Uiso 1 1 calc R U .
H16C H 0.2333 0.5273 0.1169 0.071 Uiso 1 1 calc R U .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ir Ir -4.7710 6.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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_3
O3 Ir1 O2 175.9(7) .
O3 Ir1 O1 89.7(6) .
O2 Ir1 O1 89.7(7) .
O3 Ir1 N2 92.5(8) .
O2 Ir1 N2 83.5(7) .
O1 Ir1 N2 90.3(7) .
O3 Ir1 N1 95.1(7) .
O2 Ir1 N1 88.8(7) .
O1 Ir1 N1 83.0(7) .
N2 Ir1 N1 169.9(7) .
O3 Ir1 Cl02 91.1(4) .
O2 Ir1 Cl02 89.3(5) .
O1 Ir1 Cl02 178.3(5) .
N2 Ir1 Cl02 88.2(5) .
N1 Ir1 Cl02 98.4(5) .
C7 O1 Ir1 115.4(13) .
C15 O2 Ir1 114.9(14) .
Ir1 O3 Ir1 156.4(13) 2_655
C5 N1 C1 121.4(19) .
C5 N1 Ir1 113.1(14) .
C1 N1 Ir1 124.1(15) .
C13 N2 C9 123(2) .
C13 N2 Ir1 112.5(16) .
C9 N2 Ir1 124.0(16) .
C2 C1 N1 119(2) .
C2 C1 H1 120.3 .
N1 C1 H1 120.3 .
C1 C2 C3 122(2) .
C1 C2 H2 119.0 .
C3 C2 H2 119.0 .
C2 C3 C4 115(2) .
C2 C3 H3 122.4 .
C4 C3 H3 122.4 .
C5 C4 C3 122(2) .
C5 C4 H4 118.8 .
C3 C4 H4 118.8 .
N1 C5 C4 119(2) .
N1 C5 C7 117.5(19) .
C4 C5 C7 123(2) .
C7 C6 H6A 109.5 .
C7 C6 H6B 109.5 .
H6A C6 H6B 109.5 .
C7 C6 H6C 109.5 .
H6A C6 H6C 109.5 .
H6B C6 H6C 109.5 .
O1 C7 C8 107.9(18) .
O1 C7 C5 110.6(17) .
C8 C7 C5 111(2) .
O1 C7 C6 108.6(18) .
C8 C7 C6 111.3(18) .
C5 C7 C6 107.6(18) .
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 .
N2 C9 C10 118(2) .
N2 C9 H9 120.8 .
C10 C9 H9 120.8 .
C11 C10 C9 120(2) .
C11 C10 H10 120.2 .
C9 C10 H10 120.2 .
C10 C11 C12 122(2) .
C10 C11 H11 118.8 .
C12 C11 H11 118.8 .
C13 C12 C11 116(2) .
C13 C12 H12 122.0 .
C11 C12 H12 122.0 .
N2 C13 C12 120(2) .
N2 C13 C15 119(2) .
C12 C13 C15 121(2) .
C15 C14 H14A 109.5 .
C15 C14 H14B 109.5 .
H14A C14 H14B 109.5 .
C15 C14 H14C 109.5 .
H14A C14 H14C 109.5 .
H14B C14 H14C 109.5 .
O2 C15 C13 109.8(19) .
O2 C15 C14 107.9(19) .
C13 C15 C14 112(2) .
O2 C15 C16 106.2(19) .
C13 C15 C16 111(2) .
C14 C15 C16 110(2) .
C15 C16 H16A 109.5 .
C15 C16 H16B 109.5 .
H16A C16 H16B 109.5 .
C15 C16 H16C 109.5 .
H16A C16 H16C 109.5 .
H16B C16 H16C 109.5 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ir1 O3 1.917(5) .
Ir1 O2 1.940(16) .
Ir1 O1 1.948(15) .
Ir1 N2 2.036(18) .
Ir1 N1 2.045(17) .
Ir1 Cl02 2.365(5) .
O1 C7 1.44(3) .
O2 C15 1.46(3) .
O3 Ir1 1.917(5) 2_655
N1 C5 1.32(3) .
N1 C1 1.40(3) .
N2 C13 1.31(3) .
N2 C9 1.38(3) .
C1 C2 1.33(3) .
C1 H1 0.9300 .
C2 C3 1.40(4) .
C2 H2 0.9300 .
C3 C4 1.41(3) .
C3 H3 0.9300 .
C4 C5 1.36(3) .
C4 H4 0.9300 .
C5 C7 1.53(3) .
C6 C7 1.57(3) .
C6 H6A 0.9600 .
C6 H6B 0.9600 .
C6 H6C 0.9600 .
C7 C8 1.52(3) .
C8 H8A 0.9600 .
C8 H8B 0.9600 .
C8 H8C 0.9600 .
C9 C10 1.39(3) .
C9 H9 0.9300 .
C10 C11 1.34(4) .
C10 H10 0.9300 .
C11 C12 1.42(4) .
C11 H11 0.9300 .
C12 C13 1.42(3) .
C12 H12 0.9300 .
C13 C15 1.50(3) .
C14 C15 1.50(3) .
C14 H14A 0.9600 .
C14 H14B 0.9600 .
C14 H14C 0.9600 .
C15 C16 1.56(3) .
C16 H16A 0.9600 .
C16 H16B 0.9600 .
C16 H16C 0.9600 .
