Probing the Oxidation Chemistry of Half-Sandwich Iridium Complexes with Oxygen Atom Transfer Reagents
Christopher R. Turlington; Daniel P. Harrison; Peter S. White; Maurice Brookhart; Joseph L. Templeton; Inorganic Chemistry 52 (2013) 11351–11360; doi:10.1021/ic4016405

data_4336250
_publ_contact_author_name
;
;
_publ_section_title
;
 Probing the Oxidation Chemistry of Half-Sandwich Iridium Complexes with
 Oxygen Atom Transfer Reagents
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11351
_journal_page_last               11360
_journal_paper_doi               10.1021/ic4016405
_journal_volume                  52
_journal_year                    2013
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C42 H46 Ag Ir2 N2, C F3 O3 S'
_chemical_formula_sum            'C43 H46 Ag F3 Ir2 N2 O3 S'
_chemical_formula_weight         1220.22
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_primary     iterative
_audit_creation_date             2013-06-25
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_cell_angle_alpha                90
_cell_angle_beta                 101.345(1)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.5002(2)
_cell_length_b                   24.2243(5)
_cell_length_c                   12.2503(2)
_cell_measurement_reflns_used    9936
_cell_measurement_temperature    100
_cell_measurement_theta_max      69.45
_cell_measurement_theta_min      3.65
_cell_volume                     2473.19(9)
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
olex2.refine (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_computing_structure_solution
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_av_unetI/netI     0.0394
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            18010
_diffrn_reflns_theta_full        66.500000
_diffrn_reflns_theta_max         69.84
_diffrn_reflns_theta_min         3.65
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    14.121
_exptl_absorpt_correction_T_max  0.4682
_exptl_absorpt_correction_T_min  0.2246
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
R(int) was 0.1098 before and 0.0448 after correction.
The Ratio of minimum to maximum transmission is 0.4797.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.6384
_exptl_crystal_description       plate
_exptl_crystal_F_000             1172
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.909893
_refine_diff_density_min         -0.808455
_refine_diff_density_rms         0.147682
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   0.46(2)
_refine_ls_d_res_high            0.821193
_refine_ls_d_res_low             12.112150
_refine_ls_goodness_of_fit_ref   1.043320
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    73
_refine_ls_number_parameters     510
_refine_ls_number_reflns         8193
_refine_ls_number_restraints     110
_refine_ls_restrained_S_all      1.036380
_refine_ls_R_factor_all          0.036109
_refine_ls_R_factor_gt           0.035448
_refine_ls_shift/su_max          0.0056
_refine_ls_shift/su_mean         0.0004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0529P)^2^+7.1219P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.094271
_reflns_Friedel_coverage         0.773
_reflns_limit_h_max              9
_reflns_limit_h_min              -9
_reflns_limit_k_max              29
_reflns_limit_k_min              -28
_reflns_limit_l_max              14
_reflns_limit_l_min              -14
_reflns_number_gt                4679
_reflns_number_total             4801
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ic4016405_si_003.cif
_cod_data_source_block           x1111013
_cod_database_code               4336250
_olex2_refinement_description
;
1. others
 Fixed Sof: O2(0.5) O4(0.5) O1(0.5) O6(0.5) O3(0.5) O5(0.5)
 Fixed X: H1(0.1153) H2(0.0528) H3(0.2492) H4(0.533) H7(0.7627) H8(1.0153)
 H9(1.0159) H10(0.7863) H17a(0.6577) H17b(0.7361) H17c(0.6577) H18a(0.257)
 H18b(0.4215) H18c(0.2563) H19a(-0.0113) H19b(0.029) H19c(-0.0099) H20a(0.2644)
 H20b(0.0964) H20c(0.2055) H21a(0.675) H21b(0.542) H21c(0.541) H22(0.8889)
 H23(0.9476) H24(0.7278) H25(0.4883) H28(0.2329) H29(-0.0011) H30(-0.0133)
 H31(0.2272) H38a(0.9821) H38b(1.0118) H38c(1.0226) H39a(0.9109) H39b(0.8412)
 H39c(0.7454) H40a(0.4526) H40b(0.3279) H40c(0.4539) H41a(0.2882) H41b(0.3822)
 H41c(0.342) H42a(0.6005) H42b(0.7865) H42c(0.7251)
 Fixed Y: H1(0.6911) H2(0.7767) H3(0.8408) H4(0.8149) H7(0.7859) H8(0.748)
 H9(0.6596) H10(0.6103) H17a(0.5693) H17b(0.5494) H17c(0.5052) H18a(0.6251)
 H18b(0.5957) H18c(0.5622) H19a(0.5932) H19b(0.6065) H19c(0.5445) H20a(0.5515)
 H20b(0.5485) H20c(0.4944) H21a(0.514) H21b(0.5173) H21c(0.467) H22(0.5891)
 H23(0.5021) H24(0.4432) H25(0.4617) H28(0.4946) H29(0.5322) H30(0.6218)
 H31(0.6744) H38a(0.6791) H38b(0.6832) H38c(0.7375) H39a(0.7672) H39b(0.712)
 H39c(0.769) H40a(0.758) H40b(0.7621) H40c(0.8109) H41a(0.7135) H41b(0.7265)
 H41c(0.7754) H42a(0.6773) H42b(0.6677) H42c(0.7273)
 Fixed Z: H1(-0.3392) H2(-0.4165) H3(-0.419) H4(-0.3437) H7(-0.2537) H8(-
 0.1627) H9(-0.0861) H10(-0.1041) H17a(-0.3906) H17b(-0.2673) H17c(-0.3591)
 H18a(-0.4948) H18b(-0.5065) H18c(-0.5348) H19a(-0.2858) H19b(-0.4053) H19c(-
 0.3739) H20a(-0.0319) H20b(-0.1178) H20c(-0.0918) H21a(-0.1045) H21b(-0.0289)
 H21c(-0.1139) H22(0.3495) H23(0.4315) H24(0.4407) H25(0.3467) H28(0.2643)
 H29(0.1682) H30(0.1055) H31(0.114) H38a(0.4209) H38b(0.2961) H38c(0.3717)
 H39a(0.1445) H39b(0.081) H39c(0.0558) H40a(0.0381) H40b(0.1201) H40c(0.1166)
 H41a(0.3074) H41b(0.4313) H41c(0.3424) H42a(0.5133) H42b(0.5123) H42c(0.5418)
;