#------------------------------------------------------------------------------
#$Date: 2016-03-21 06:43:43 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178531 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/36/4063640.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_4063640
loop_
_publ_author_name
'Yang, Wei'
'Fu, Hao'
'Song, Qijun'
'Zhang, Min'
'Ding, Yuqiang'
_publ_section_title
;
 Amidate Iridium(III) Bis(2-pyridyl)phenyl Complexes: Application Examples
 of Amidate Ancillary Ligands in Iridium(III)-Cyclometalated Complexes
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              77
_journal_paper_doi               10.1021/om100714g
_journal_volume                  30
_journal_year                    2011
_chemical_formula_sum            'C30 H24 Ir N3 O'
_chemical_formula_weight         634.72
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.995(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.402(3)
_cell_length_b                   16.964(5)
_cell_length_c                   13.984(4)
_cell_measurement_reflns_used    11972
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      25.10
_cell_measurement_theta_min      1.89
_cell_volume                     2461.6(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0804
_diffrn_reflns_av_sigmaI/netI    0.1114
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11972
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    5.452
_exptl_absorpt_correction_T_max  0.6036
_exptl_absorpt_correction_T_min  0.3569
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.713
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         4.608
_refine_diff_density_min         -2.869
_refine_diff_density_rms         0.256
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.852
_refine_ls_hydrogen_treatment    refine
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         4376
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.852
_refine_ls_R_factor_all          0.1036
_refine_ls_R_factor_gt           0.0679
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1082P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1598
_refine_ls_wR_factor_ref         0.1689
_reflns_number_gt                2371
_reflns_number_total             4376
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100714g_si_001.cif
_cod_data_source_block           xb1959m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        2461.6(11)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4063640
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Ir1 Ir -0.01235(5) 0.22896(3) 0.51544(3) 0.0523(2) Uani 1 1 d .
O1 O 0.0124(9) 0.1866(6) 0.3642(5) 0.066(2) Uani 1 1 d .
N1 N 0.0626(10) 0.1269(6) 0.5642(7) 0.050(3) Uani 1 1 d .
N2 N -0.0942(11) 0.3326(6) 0.4754(9) 0.073(3) Uani 1 1 d .
N3 N 0.1536(11) 0.2637(7) 0.4426(8) 0.066(3) Uani 1 1 d .
C1 C 0.1846(14) 0.1025(8) 0.5599(9) 0.068(4) Uani 1 1 d .
H1 H 0.2426 0.1370 0.5344 0.082 Uiso 1 1 calc R
C2 C 0.2307(16) 0.0290(9) 0.5910(9) 0.074(4) Uani 1 1 d .
H2 H 0.3158 0.0143 0.5845 0.089 Uiso 1 1 calc R
C3 C 0.1457(19) -0.0205(8) 0.6314(11) 0.080(5) Uani 1 1 d .
H3 H 0.1729 -0.0692 0.6557 0.096 Uiso 1 1 calc R
C4 C 0.0257(17) 0.0017(7) 0.6356(10) 0.070(4) Uani 1 1 d .
H4 H -0.0317 -0.0326 0.6622 0.084 Uiso 1 1 calc R
C5 C -0.0197(14) 0.0738(7) 0.6021(9) 0.060(4) Uani 1 1 d .
C6 C -0.1540(13) 0.1040(8) 0.6004(9) 0.059(3) Uani 1 1 d .
C7 C -0.2542(15) 0.0596(9) 0.6330(10) 0.077(4) Uani 1 1 d .
H7 H -0.2392 0.0097 0.6589 0.092 Uiso 1 1 calc R
C8 C -0.3752(15) 0.0910(10) 0.6264(11) 0.086(5) Uani 1 1 d .
H8 H -0.4427 0.0637 0.6515 0.104 Uiso 1 1 calc R
C9 C -0.3979(15) 0.1619(9) 0.5831(10) 0.078(4) Uani 1 1 d .
H9 H -0.4821 0.1804 0.5740 0.094 Uiso 1 1 calc R
C10 C -0.2966(14) 0.2077(8) 0.5521(9) 0.063(4) Uani 1 1 d .
H10 H -0.3132 0.2579 0.5276 0.076 Uiso 1 1 calc R
C11 C -0.1709(13) 0.1782(7) 0.5579(7) 0.050(3) Uani 1 1 d .
C12 C -0.1417(14) 0.3465(10) 0.3823(10) 0.081(5) Uani 1 1 d .
H12 H -0.1390 0.3067 0.3368 0.097 Uiso 1 1 calc R
C13 C -0.1923(18) 0.4176(12) 0.3568(14) 0.106(6) Uani 1 1 d .
H13 H -0.2236 0.4272 0.2940 0.127 Uiso 1 1 calc R
C14 C -0.1967(18) 0.4763(12) 0.4266(19) 0.108(7) Uani 1 1 d .
H14 H -0.2317 0.5254 0.4106 0.130 Uiso 1 1 calc R
C15 C -0.1505(13) 0.4618(9) 0.5167(14) 0.083(5) Uani 1 1 d .
H15 H -0.1545 0.5008 0.5631 0.100 Uiso 1 1 calc R
C16 C -0.0960(12) 0.3883(8) 0.5418(11) 0.062(4) Uani 1 1 d .
C17 C -0.0405(12) 0.3636(9) 0.6340(11) 0.067(4) Uani 1 1 d .
C18 C -0.0308(16) 0.4121(9) 0.7161(14) 0.089(5) Uani 1 1 d .
H18 H -0.0602 0.4638 0.7121 0.107 Uiso 1 1 calc R
C19 C 0.0206(17) 0.3838(12) 0.7999(14) 0.101(6) Uani 1 1 d .
H19 H 0.0263 0.4160 0.8539 0.121 Uiso 1 1 calc R
C20 C 0.0641(16) 0.3086(12) 0.8060(11) 0.089(5) Uani 1 1 d .
H20 H 0.1012 0.2900 0.8641 0.107 Uiso 1 1 calc R
C21 C 0.0548(14) 0.2598(9) 0.7292(11) 0.073(4) Uani 1 1 d .
H21 H 0.0827 0.2079 0.7365 0.088 Uiso 1 1 calc R
C22 C 0.0022(11) 0.2864(7) 0.6357(9) 0.053(3) Uani 1 1 d .
C23 C 0.2031(15) 0.2050(11) 0.2816(11) 0.108(6) Uani 1 1 d .
H23A H 0.2398 0.2528 0.2588 0.162 Uiso 1 1 calc R
H23B H 0.1479 0.1818 0.2314 0.162 Uiso 1 1 calc R
H23C H 0.2709 0.1687 0.3009 0.162 Uiso 1 1 calc R
C24 C 0.1245(14) 0.2235(8) 0.3673(10) 0.060(4) Uani 1 1 d .
C25 C 0.2647(15) 0.3063(9) 0.4647(13) 0.077(4) Uani 1 1 d .
C26 C 0.3280(19) 0.3500(10) 0.3953(14) 0.113(6) Uani 1 1 d .
H26 H 0.2964 0.3514 0.3315 0.136 Uiso 1 1 calc R
C27 C 0.442(2) 0.3916(15) 0.427(2) 0.154(13) Uani 1 1 d .
H27 H 0.4866 0.4182 0.3818 0.184 Uiso 1 1 calc R
C28 C 0.490(3) 0.3949(17) 0.521(3) 0.178(18) Uani 1 1 d .
H28 H 0.5638 0.4233 0.5386 0.214 Uiso 1 1 calc R
C29 C 0.4236(18) 0.3545(11) 0.5872(18) 0.121(8) Uani 1 1 d .
H29 H 0.4529 0.3567 0.6515 0.145 Uiso 1 1 calc R
C30 C 0.3135(15) 0.3104(10) 0.5600(13) 0.085(4) Uani 1 1 d .
H30 H 0.2718 0.2831 0.6066 0.102 Uiso 1 1 calc 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'
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
C22 Ir1 C11 88.5(4)
C22 Ir1 N1 97.7(5)
C11 Ir1 N1 80.5(5)
C22 Ir1 N2 79.0(5)
C11 Ir1 N2 96.8(5)
N1 Ir1 N2 175.8(4)
C22 Ir1 N3 104.9(5)
C11 Ir1 N3 166.4(4)
N1 Ir1 N3 95.3(4)
N2 Ir1 N3 88.1(5)
C22 Ir1 O1 164.0(4)
C11 Ir1 O1 107.0(4)
N1 Ir1 O1 88.7(3)
N2 Ir1 O1 95.2(4)
N3 Ir1 O1 59.8(4)
C24 O1 Ir1 88.6(7)
C1 N1 C5 115.5(11)
C1 N1 Ir1 126.9(9)
C5 N1 Ir1 117.5(8)
C16 N2 C12 121.1(13)
C16 N2 Ir1 117.0(10)
C12 N2 Ir1 121.8(10)
C24 N3 C25 127.7(13)
C24 N3 Ir1 95.3(9)
C25 N3 Ir1 136.6(10)
N1 C1 C2 124.7(14)
C3 C2 C1 117.3(15)
C4 C3 C2 119.1(14)
C3 C4 C5 123.0(16)
N1 C5 C4 120.3(14)
N1 C5 C6 112.2(11)
C4 C5 C6 127.5(14)
C7 C6 C11 123.5(13)
C7 C6 C5 122.3(13)
C11 C6 C5 114.1(11)
C8 C7 C6 118.5(14)
C9 C8 C7 120.5(14)
C8 C9 C10 121.1(14)
C11 C10 C9 120.4(13)
C10 C11 C6 115.9(12)
C10 C11 Ir1 128.4(10)
C6 C11 Ir1 115.7(10)
C13 C12 N2 120.5(17)
C12 C13 C14 118.8(19)
C15 C14 C13 119.9(18)
C14 C15 C16 120.8(18)
N2 C16 C15 118.9(15)
N2 C16 C17 113.3(12)
C15 C16 C17 127.8(15)
C22 C17 C18 122.3(15)
C22 C17 C16 113.6(13)
C18 C17 C16 124.2(15)
C19 C18 C17 120.3(16)
C18 C19 C20 120.1(16)
C21 C20 C19 121.4(17)
C20 C21 C22 121.7(15)
C17 C22 C21 114.2(12)
C17 C22 Ir1 117.1(11)
C21 C22 Ir1 128.7(10)
N3 C24 O1 116.1(12)
N3 C24 C23 130.5(14)
O1 C24 C23 113.3(14)
N3 C25 C30 118.9(14)
N3 C25 C26 122.9(17)
C30 C25 C26 118.2(17)
C25 C26 C27 117(2)
C28 C27 C26 124(3)
C27 C28 C29 118(3)
C28 C29 C30 121(2)
C25 C30 C29 121.5(18)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Ir1 C22 1.940(12)
Ir1 C11 1.988(13)
Ir1 N1 1.999(10)
Ir1 N2 2.016(11)
Ir1 N3 2.146(11)
Ir1 O1 2.266(7)
O1 C24 1.322(16)
N1 C1 1.340(16)
N1 C5 1.374(16)
N2 C16 1.326(16)
N2 C12 1.380(16)
N3 C24 1.273(17)
N3 C25 1.380(18)
C1 C2 1.394(18)
C2 C3 1.37(2)
C3 C4 1.31(2)
C4 C5 1.380(16)
C5 C6 1.487(18)
C6 C7 1.389(18)
C6 C11 1.399(16)
C7 C8 1.364(19)
C8 C9 1.360(19)
C9 C10 1.401(19)
C10 C11 1.397(17)
C12 C13 1.35(2)
C13 C14 1.40(2)
C14 C15 1.34(2)
C15 C16 1.403(19)
C16 C17 1.438(18)
C17 C22 1.383(17)
C17 C18 1.41(2)
C18 C19 1.34(2)
C19 C20 1.36(2)
C20 C21 1.353(19)
C21 C22 1.454(19)
C23 C24 1.529(19)
C25 C30 1.39(2)
C25 C26 1.42(2)
C26 C27 1.42(3)
C27 C28 1.36(4)
C28 C29 1.38(4)
C29 C30 1.40(2)
