#------------------------------------------------------------------------------
#$Date: 2019-11-25 10:46:14 +0200 (Mon, 25 Nov 2019) $
#$Revision: 240700 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/01/4130140.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_4130140
loop_
_publ_author_name
'Chen, Tsun-Ren'
'Wu, Fang-Siou'
'Lee, Hsiu-Pen'
'Chen, Kelvin H.-C.'
_publ_section_title
;
 Diiridium Bimetallic Complexes Function as a Redox Switch To Directly
 Split Carbonate into Carbon Monoxide and Oxygen.
;
_journal_issue                   11
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3643
_journal_page_last               3646
_journal_paper_doi               10.1021/jacs.6b00715
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C52 H24 F8 Ir2 N4 O6, 2(C H2 Cl2)'
_chemical_formula_sum            'C54 H28 Cl4 F8 Ir2 N4 O6'
_chemical_formula_weight         1507.00
_space_group_IT_number           68
_space_group_name_Hall           '-C 2a 2ac'
_space_group_name_H-M_alt        'C c c a :2'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      68
_symmetry_space_group_name_H-M   'C c c a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.2793(4)
_cell_length_b                   16.5304(5)
_cell_length_c                   23.6000(8)
_cell_measurement_reflns_used    9812
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.39
_cell_measurement_theta_min      3.01
_cell_volume                     5570.6(3)
_computing_cell_refinement       'SAINT V7.34A (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2010)'
_computing_data_reduction        'SAINT V7.34A (Bruker AXS, 2006)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_sigmaI/netI    0.0190
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            32520
_diffrn_reflns_theta_full        26.42
_diffrn_reflns_theta_max         26.42
_diffrn_reflns_theta_min         3.20
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    5.043
_exptl_absorpt_correction_T_max  0.4320
_exptl_absorpt_correction_T_min  0.2050
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            red
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             2888
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_platon_squeeze_details          ' '
_refine_diff_density_max         0.909
_refine_diff_density_min         -1.780
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.159
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         2863
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.159
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0406
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0226P)²+66.0135P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0796
_refine_ls_wR_factor_ref         0.0842
_reflns_number_gt                2353
_reflns_number_total             2863
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja6b00715_si_002.cif
_cod_data_source_block           irfpboco3
_cod_original_sg_symbol_H-M      'C c c a'
_cod_database_code               4130140
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z'
'-x, y, -z+1/2'
'x+1/2, -y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1, -y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'x+1, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z'
'x, -y, z-1/2'
'-x-1/2, y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x, y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
'-x, 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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Ir Ir 0.880657(17) 0.2500 0.2500 0.03021(11) Uani 1 2 d S
F1 F 0.5756(3) 0.4977(3) 0.1813(3) 0.0882(16) Uani 1 1 d .
F2 F 0.7371(3) 0.3726(3) 0.3293(2) 0.0738(15) Uani 1 1 d .
O1 O 0.8076(3) 0.2939(3) 0.0844(2) 0.0488(12) Uani 1 1 d .
O2 O 1.0000 0.1694(3) 0.2500 0.0254(10) Uani 1 2 d S
N N 0.8736(3) 0.2459(3) 0.1635(2) 0.0358(11) Uani 1 1 d .
C1 C 0.9062(4) 0.1989(3) 0.1188(3) 0.0350(14) Uani 1 1 d .
C2 C 0.9644(4) 0.1324(3) 0.1151(3) 0.0382(15) Uani 1 1 d .
H2A H 0.9926 0.1087 0.1476 0.046 Uiso 1 1 d R
C3 C 0.9817(4) 0.1009(4) 0.0620(3) 0.0485(18) Uani 1 1 d .
H3A H 1.0221 0.0556 0.0583 0.058 Uiso 1 1 calc R
C4 C 0.9410(5) 0.1343(4) 0.0134(4) 0.056(2) Uani 1 1 d .
H4A H 0.9548 0.1112 -0.0225 0.067 Uiso 1 1 calc R
C5 C 0.8811(5) 0.2002(5) 0.0163(3) 0.0527(19) Uani 1 1 d .
H5A H 0.8530 0.2231 -0.0165 0.063 Uiso 1 1 calc R
C6 C 0.8653(4) 0.2301(4) 0.0696(3) 0.0446(17) Uani 1 1 d .
C7 C 0.8155(4) 0.2986(4) 0.1413(3) 0.0447(18) Uani 1 1 d .
C8 C 0.7615(4) 0.3503(4) 0.1778(3) 0.0492(19) Uani 1 1 d .
C9 C 0.6946(5) 0.4049(4) 0.1578(4) 0.063(2) Uani 1 1 d .
H9A H 0.6842 0.4133 0.1185 0.076 Uiso 1 1 calc R
C10 C 0.6446(6) 0.4455(5) 0.1987(5) 0.0882(16) Uani 1 1 d .
C11 C 0.6576(5) 0.4355(4) 0.2553(4) 0.069(3) Uani 1 1 d .
H11A H 0.6210 0.4645 0.2821 0.083 Uiso 1 1 calc R
C12 C 0.7260(4) 0.3815(4) 0.2725(4) 0.059(2) Uani 1 1 d .
C13 C 0.7809(4) 0.3345(4) 0.2367(3) 0.0454(19) Uani 1 1 d .
Cl Cl 0.8163(2) 0.4340(2) 0.97785(17) 0.1447(17) Uani 1 1 d .
C14 C 0.7500 0.5000 0.9386(5) 0.069(3) Uani 1 2 d S
H14A H 0.7091 0.4693 0.9146 0.082 Uiso 1 1 d R
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'
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'
F F 0.0171 0.0103 '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'
Ir Ir -1.4442 7.9887 '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_1
_geom_angle_site_symmetry_3
C13 Ir C13 90.3(3) . 8_455
C13 Ir N 95.6(2) . 8_455
C13 Ir N 80.4(3) 8_455 8_455
C13 Ir N 80.4(3) . .
C13 Ir N 95.6(2) 8_455 .
N Ir N 174.3(2) 8_455 .
C13 Ir O2 169.00(19) . .
C13 Ir O2 97.47(19) 8_455 .
N Ir O2 93.40(12) 8_455 .
N Ir O2 91.06(12) . .
C13 Ir O2 97.47(19) . 6_655
C13 Ir O2 169.00(19) 8_455 6_655
N Ir O2 91.06(12) 8_455 6_655
N Ir O2 93.40(12) . 6_655
O2 Ir O2 76.0(2) . 6_655
C7 O1 C6 104.2(5) . .
Ir O2 Ir 104.0(2) . 6_655
C7 N C1 106.2(6) . .
C7 N Ir 114.1(5) . .
C1 N Ir 139.4(4) . .
C2 C1 N 134.0(6) . .
C2 C1 C6 119.5(6) . .
N C1 C6 106.5(5) . .
C3 C2 C1 117.7(6) . .
C2 C3 C4 121.5(7) . .
C5 C4 C3 121.8(8) . .
C6 C5 C4 115.4(6) . .
C5 C6 O1 127.2(6) . .
C5 C6 C1 124.1(6) . .
O1 C6 C1 108.7(6) . .
N C7 O1 114.4(6) . .
N C7 C8 119.6(7) . .
O1 C7 C8 125.8(5) . .
C9 C8 C13 125.1(7) . .
C9 C8 C7 123.2(8) . .
C13 C8 C7 111.5(5) . .
C10 C9 C8 115.6(8) . .
C11 C10 C9 124.0(7) . .
C11 C10 F1 117.9(9) . .
C9 C10 F1 118.0(10) . .
C10 C11 C12 117.6(8) . .
F2 C12 C11 116.2(7) . .
F2 C12 C13 118.3(5) . .
C11 C12 C13 125.5(9) . .
C8 C13 C12 112.1(6) . .
C8 C13 Ir 114.3(5) . .
C12 C13 Ir 133.6(6) . .
Cl C14 Cl 114.7(8) 2_665 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ir C13 2.020(5) .
Ir C13 2.020(5) 8_455
Ir N 2.044(5) 8_455
Ir N 2.044(5) .
Ir O2 2.163(3) .
Ir O2 2.163(3) 6_655
F1 C10 1.372(8) .
F2 C12 1.358(10) .
O1 C7 1.350(9) .
O1 C6 1.383(8) .
O2 Ir 2.163(3) 6_655
N C7 1.312(7) .
N C1 1.391(8) .
C1 C2 1.381(8) .
C1 C6 1.400(9) .
C2 C3 1.380(10) .
C3 C4 1.398(10) .
C4 C5 1.387(10) .
C5 C6 1.370(10) .
C7 C8 1.439(10) .
C8 C9 1.396(8) .
C8 C13 1.441(10) .
C9 C10 1.375(14) .
C10 C11 1.360(14) .
C11 C12 1.384(8) .
C12 C13 1.390(10) .
Cl C14 1.715(7) .
C14 Cl 1.715(7) 2_665
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.250 0.750 207 37 ' '
2 0.000 0.750 0.250 207 38 ' '
3 0.500 0.250 0.250 207 38 ' '
4 0.500 0.750 0.750 207 37 ' '
