#------------------------------------------------------------------------------
#$Date: 2016-03-26 02:56:09 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180161 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/57/7105735.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_7105735
loop_
_publ_author_name
'Arianna Savini'
'Gianfranco Bellachioma'
'Gianluca Ciancaleoni'
'Cristiano Zuccaccia'
'Daniele Zuccaccia'
'Alceo Macchioni'
_publ_section_title
;
 Iridium(III) Molecular Catalysts for Water Oxidation: the Simpler the
 Faster
;
_journal_name_full               Chem.Commun.
_journal_page_first              9218
_journal_paper_doi               10.1039/c0cc03801f
_journal_volume                  46
_journal_year                    2010
_chemical_formula_moiety         'C22 H23 Ir N2 O4'
_chemical_formula_sum            'C22 H23 Ir N2 O4'
_chemical_formula_weight         571.62
_chemical_name_common            '[(Cp*)Ir(2-bzpy)NO3]'
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000
_cell_angle_beta                 101.606(8)
_cell_angle_gamma                90.000
_cell_formula_units_Z            4
_cell_length_a                   14.112(7)
_cell_length_b                   9.453(5)
_cell_length_c                   15.848(6)
_cell_measurement_reflns_used    13855
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      29.2337
_cell_measurement_theta_min      3.8989
_cell_volume                     2070.9(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 8.2492
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type
'Goniometer KM4/Xcalibur, detector: Sapphire2'
_diffrn_measurement_method       'ω and π scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0299
_diffrn_reflns_av_sigmaI/netI    0.0260
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            26915
_diffrn_reflns_theta_full        29.30
_diffrn_reflns_theta_max         29.30
_diffrn_reflns_theta_min         3.91
_exptl_absorpt_coefficient_mu    6.478
_exptl_absorpt_correction_T_max  0.40267
_exptl_absorpt_correction_T_min  0.28049
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.32 (release 27-01-2009 CrysAlis171 .NET)
(compiled Jan 27 2009,14:17:37)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.833
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       prism
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.809
_refine_diff_density_min         -0.997
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         4996
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0313
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0308P)²+4.5613P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0689
_refine_ls_wR_factor_ref         0.0769
_reflns_number_gt                3552
_reflns_number_total             5612
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0CC03801F.TXT
_cod_data_source_block           '[(Cp*)Ir(2-bzpy)NO3]'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7105735
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'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
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6450(4) 0.1982(5) 1.0018(3) 0.0490(9) Uani 1 1 d . . .
C2 C 0.6353(4) 0.2269(6) 1.0823(4) 0.0579(14) Uani 1 1 d . . .
H2 H 0.6902 0.2463 1.1240 0.084(8) Uiso 1 1 calc R . .
C3 C 0.5460(6) 0.2285(7) 1.1048(5) 0.0778(14) Uani 1 1 d . . .
H3 H 0.5413 0.2479 1.1614 0.084(8) Uiso 1 1 calc R . .
C4 C 0.4641(6) 0.2018(7) 1.0445(4) 0.0778(14) Uani 1 1 d . . .
H4 H 0.4036 0.2042 1.0592 0.084(8) Uiso 1 1 calc R . .
C5 C 0.4730(5) 0.1711(7) 0.9610(4) 0.0682(16) Uani 1 1 d . . .
H5 H 0.4187 0.1517 0.9187 0.084(8) Uiso 1 1 calc R . .
C6 C 0.5649(4) 0.1700(5) 0.9418(3) 0.0490(9) Uani 1 1 d . . .
C7 C 0.5719(4) 0.1249(6) 0.8516(3) 0.0532(13) Uani 1 1 d . . .
C8 C 0.6553(5) 0.0429(6) 0.8369(3) 0.0581(9) Uani 1 1 d . . .
C9 C 0.6387(5) -0.0590(6) 0.7714(3) 0.0631(16) Uani 1 1 d . . .
H9 H 0.5774 -0.0671 0.7367 0.084(8) Uiso 1 1 calc R . .
C10 C 0.7108(6) -0.1465(6) 0.7576(4) 0.0718(18) Uani 1 1 d . . .
H10 H 0.6986 -0.2161 0.7153 0.084(8) Uiso 1 1 calc R . .
C11 C 0.8026(5) -0.1299(6) 0.8077(4) 0.0710(17) Uani 1 1 d . . .
H11 H 0.8524 -0.1887 0.7988 0.084(8) Uiso 1 1 calc R . .
C12 C 0.8209(5) -0.0278(6) 0.8705(4) 0.0629(15) Uani 1 1 d . . .
H12 H 0.8834 -0.0174 0.9025 0.084(8) Uiso 1 1 calc R . .
C13 C 0.7706(5) 0.4171(6) 0.9042(4) 0.0685(18) Uani 1 1 d . . .
C14 C 0.7897(5) 0.4548(6) 0.9938(4) 0.0639(16) Uani 1 1 d . . .
C15 C 0.8773(5) 0.3978(6) 1.0335(3) 0.0594(15) Uani 1 1 d . . .
C16 C 0.9175(4) 0.3273(6) 0.9694(3) 0.0546(13) Uani 1 1 d . . .
C17 C 0.8540(5) 0.3444(6) 0.8889(3) 0.0616(16) Uani 1 1 d . . .
C18 C 0.6882(7) 0.4710(9) 0.8369(7) 0.149(5) Uani 1 1 d . . .
H18A H 0.6907 0.5724 0.8350 0.171(11) Uiso 1 1 calc R . .
H18B H 0.6280 0.4419 0.8510 0.171(11) Uiso 1 1 calc R . .
H18C H 0.6930 0.4332 0.7818 0.171(11) Uiso 1 1 calc R . .
C19 C 0.7235(7) 0.5461(9) 1.0346(7) 0.141(4) Uani 1 1 d . . .
H19A H 0.7390 0.5343 1.0960 0.171(11) Uiso 1 1 calc R . .
H19B H 0.6576 0.5185 1.0132 0.171(11) Uiso 1 1 calc R . .
H19C H 0.7318 0.6434 1.0205 0.171(11) Uiso 1 1 calc R . .
C20 C 0.9265(7) 0.4071(9) 1.1273(4) 0.114(3) Uani 1 1 d . . .
H20A H 0.9706 0.4857 1.1354 0.171(11) Uiso 1 1 calc R . .
H20B H 0.9616 0.3213 1.1442 0.171(11) Uiso 1 1 calc R . .
H20C H 0.8787 0.4204 1.1620 0.171(11) Uiso 1 1 calc R . .
C21 C 1.0162(5) 0.2560(8) 0.9866(7) 0.101(3) Uani 1 1 d . . .
H21A H 1.0161 0.1801 0.9463 0.171(11) Uiso 1 1 calc R . .
H21B H 1.0299 0.2191 1.0442 0.171(11) Uiso 1 1 calc R . .
H21C H 1.0648 0.3239 0.9801 0.171(11) Uiso 1 1 calc R . .
C22 C 0.8725(8) 0.2965(8) 0.8033(4) 0.113(3) Uani 1 1 d . . .
H22A H 0.8860 0.3772 0.7709 0.171(11) Uiso 1 1 calc R . .
H22B H 0.8165 0.2482 0.7721 0.171(11) Uiso 1 1 calc R . .
H22C H 0.9270 0.2336 0.8123 0.171(11) Uiso 1 1 calc R . .
O1 O 0.5025(3) 0.1469(6) 0.7934(3) 0.0819(13) Uani 1 1 d . . .
O2A O 0.8471(5) 0.0846(5) 1.0747(3) 0.0561(14) Uani 0.70 1 d P . .
O3A O 0.7398(5) -0.0834(7) 1.0562(5) 0.097(2) Uani 0.70 1 d P . .
O4 O 0.8576(4) -0.0952(5) 1.1602(3) 0.0972(16) Uani 1 1 d . . .
Ir Ir 0.780817(16) 0.22393(2) 0.973044(11) 0.04609(8) Uani 1 1 d . . .
N1 N 0.7479(4) 0.0607(5) 0.8872(3) 0.0581(9) Uani 1 1 d . . .
N2 N 0.8213(5) -0.0298(6) 1.1007(3) 0.0794(18) Uani 1 1 d . . .
O3B O 0.9220(16) 0.040(2) 1.1034(13) 0.113(6) Uiso 0.30 1 d P . .
O2B O 0.7795(14) 0.056(2) 1.0725(10) 0.081(5) Uiso 0.30 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'
O O 0.0106 0.0060 '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'
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
C2 C1 C6 118.7(5) . . ?
C2 C1 Ir 117.5(4) . . ?
C6 C1 Ir 123.3(4) . . ?
C1 C2 C3 121.5(6) . . ?
C4 C3 C2 120.4(7) . . ?
C3 C4 C5 118.7(7) . . ?
C6 C5 C4 118.6(6) . . ?
C1 C6 C5 122.0(5) . . ?
C1 C6 C7 121.1(5) . . ?
C5 C6 C7 116.7(5) . . ?
O1 C7 C8 121.2(5) . . ?
O1 C7 C6 118.1(5) . . ?
C8 C7 C6 120.3(5) . . ?
N1 C8 C9 120.2(6) . . ?
N1 C8 C7 122.3(5) . . ?
C9 C8 C7 117.5(6) . . ?
C10 C9 C8 121.2(6) . . ?
C9 C10 C11 118.7(6) . . ?
C12 C11 C10 120.9(6) . . ?
C11 C12 N1 121.4(6) . . ?
C17 C13 C14 106.9(5) . . ?
C17 C13 C18 126.3(7) . . ?
C14 C13 C18 125.6(8) . . ?
C17 C13 Ir 72.5(3) . . ?
C14 C13 Ir 74.0(3) . . ?
C18 C13 Ir 128.4(5) . . ?
C15 C14 C13 109.1(5) . . ?
C15 C14 C19 127.1(7) . . ?
C13 C14 C19 123.8(7) . . ?
C15 C14 Ir 72.6(3) . . ?
C13 C14 Ir 67.3(3) . . ?
C19 C14 Ir 127.4(5) . . ?
C14 C15 C16 107.8(5) . . ?
C14 C15 C20 128.2(7) . . ?
C16 C15 C20 124.0(7) . . ?
C14 C15 Ir 71.1(3) . . ?
C16 C15 Ir 69.2(3) . . ?
C20 C15 Ir 126.0(4) . . ?
C17 C16 C15 108.7(5) . . ?
C17 C16 C21 127.1(6) . . ?
C15 C16 C21 124.1(6) . . ?
C17 C16 Ir 70.8(3) . . ?
C15 C16 Ir 73.1(3) . . ?
C21 C16 Ir 125.5(4) . . ?
C16 C17 C13 107.3(5) . . ?
C16 C17 C22 125.9(7) . . ?
C13 C17 C22 126.8(6) . . ?
C16 C17 Ir 71.2(3) . . ?
C13 C17 Ir 68.7(3) . . ?
C22 C17 Ir 126.1(4) . . ?
O2B O2A O3B 136.3(16) . . ?
O2B O2A N2 55.0(11) . . ?
O3B O2A N2 81.5(12) . . ?
O2B O2A Ir 82.4(11) . . ?
O3B O2A Ir 139.0(11) . . ?
N2 O2A Ir 132.4(5) . . ?
N1 Ir C1 87.8(2) . . ?
N1 Ir C13 109.0(2) . . ?
C1 Ir C13 104.2(2) . . ?
N1 Ir O2A 92.4(2) . . ?
C1 Ir O2A 92.6(2) . . ?
C13 Ir O2A 153.0(2) . . ?
N1 Ir C17 93.42(18) . . ?
C1 Ir C17 140.7(2) . . ?
C13 Ir C17 38.8(2) . . ?
O2A Ir C17 126.5(2) . . ?
N1 Ir C16 113.9(2) . . ?
C1 Ir C16 157.5(2) . . ?
C13 Ir C16 64.3(2) . . ?
O2A Ir C16 92.4(2) . . ?
C17 Ir C16 38.0(2) . . ?
N1 Ir C14 147.4(2) . . ?
C1 Ir C14 96.3(2) . . ?
C13 Ir C14 38.7(2) . . ?
O2A Ir C14 119.5(2) . . ?
C17 Ir C14 63.4(2) . . ?
C16 Ir C14 62.3(2) . . ?
N1 Ir C15 151.7(2) . . ?
C1 Ir C15 120.4(2) . . ?
C13 Ir C15 63.7(2) . . ?
O2A Ir C15 89.6(2) . . ?
C17 Ir C15 63.31(19) . . ?
C16 Ir C15 37.8(2) . . ?
C14 Ir C15 36.3(2) . . ?
N1 Ir O2B 84.3(5) . . ?
C1 Ir O2B 67.8(5) . . ?
C13 Ir O2B 164.7(5) . . ?
O2A Ir O2B 25.9(5) . . ?
C17 Ir O2B 151.4(5) . . ?
C16 Ir O2B 118.1(5) . . ?
C14 Ir O2B 127.1(5) . . ?
C15 Ir O2B 108.1(5) . . ?
C12 N1 C8 117.5(5) . . ?
C12 N1 Ir 120.1(4) . . ?
C8 N1 Ir 122.1(4) . . ?
O2B N2 O4 151.5(11) . . ?
O2B N2 O2A 50.2(10) . . ?
O4 N2 O2A 128.8(8) . . ?
O2B N2 O3A 73.5(12) . . ?
O4 N2 O3A 115.1(7) . . ?
O2A N2 O3A 116.1(6) . . ?
O2B N2 O3B 96.7(15) . . ?
O4 N2 O3B 87.2(9) . . ?
O2A N2 O3B 46.7(8) . . ?
O3A N2 O3B 150.0(9) . . ?
O2A O3B N2 51.8(9) . . ?
O2A O2B N2 74.8(14) . . ?
O2A O2B O3A 126.5(17) . . ?
N2 O2B O3A 62.0(11) . . ?
O2A O2B Ir 71.8(11) . . ?
N2 O2B Ir 139.8(15) . . ?
O3A O2B Ir 125.6(10) . . ?
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
C1 C2 1.337(7) . ?
C1 C6 1.349(7) . ?
C1 Ir 2.072(6) . ?
C2 C3 1.378(9) . ?
C3 C4 1.367(10) . ?
C4 C5 1.384(9) . ?
C5 C6 1.390(8) . ?
C6 C7 1.514(7) . ?
C7 O1 1.220(6) . ?
C7 C8 1.467(8) . ?
C8 N1 1.397(7) . ?
C8 C9 1.401(7) . ?
C9 C10 1.362(9) . ?
C10 C11 1.386(9) . ?
C11 C12 1.372(8) . ?
C12 N1 1.393(7) . ?
C13 C17 1.425(9) . ?
C13 C14 1.436(9) . ?
C13 C18 1.500(9) . ?
C13 Ir 2.117(5) . ?
C14 C15 1.380(8) . ?
C14 C19 1.509(9) . ?
C14 Ir 2.207(5) . ?
C15 C16 1.424(8) . ?
C15 C20 1.512(8) . ?
C15 Ir 2.225(5) . ?
C16 C17 1.413(7) . ?
C16 C21 1.522(9) . ?
C16 Ir 2.173(6) . ?
C17 C22 1.502(8) . ?
C17 Ir 2.167(5) . ?
O2A O2B 0.985(18) . ?
O2A O3B 1.15(2) . ?
O2A N2 1.237(8) . ?
O2A Ir 2.144(5) . ?
O3A N2 1.323(8) . ?
O3A O2B 1.44(2) . ?
O4 N2 1.157(6) . ?
Ir N1 2.048(5) . ?
Ir O2B 2.237(18) . ?
N2 O2B 1.051(18) . ?
N2 O3B 1.56(2) . ?
