Sequential Nitrene Transfers to an Organometallic Half-Sandwich Iridium Complex
Turlington, Christopher R.; White, Peter S.; Brookhart, Maurice; Templeton, Joseph L.; Organometallics 34 (2015) 4810–; doi:10.1021/acs.organomet.5b00717

data_4087915
_publ_section_title
;
 Sequential Nitrene Transfers to an Organometallic Half-Sandwich Iridium
 Complex
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              4810
_journal_paper_doi               10.1021/acs.organomet.5b00717
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety
'C44 H39 F6 Ir N4 O4 S2, C32 H12 B F24, C H2 Cl2'
_chemical_formula_sum            'C77 H53 B Cl2 F30 Ir N4 O4 S2'
_chemical_formula_weight         2006.26
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-08-20
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 109.2946(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.7042(4)
_cell_length_b                   17.9764(3)
_cell_length_c                   18.7177(3)
_cell_measurement_reflns_used    9756
_cell_measurement_temperature    100
_cell_measurement_theta_max      74.43
_cell_measurement_theta_min      2.46
_cell_volume                     7845.5(2)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            150642
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.546
_diffrn_reflns_theta_min         3.104
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.540
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.3132
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0831 before and 0.0530 after correction.
The Ratio of minimum to maximum transmission is 0.3132.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.699
_exptl_crystal_description       block
_exptl_crystal_F_000             3972
_exptl_crystal_size_max          0.469
_exptl_crystal_size_mid          0.273
_exptl_crystal_size_min          0.214
_refine_diff_density_max         1.242
_refine_diff_density_min         -1.612
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.249
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1241
_refine_ls_number_reflns         15861
_refine_ls_number_restraints     324
_refine_ls_restrained_S_all      1.248
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0517
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0278P)^2^+37.4036P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1227
_refine_ls_wR_factor_ref         0.1237
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15244
_reflns_number_total             15861
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00717_si_002.cif
_cod_data_source_block           x1502010
_cod_database_code               4087915
_shelx_estimated_absorpt_t_max   0.384
_shelx_estimated_absorpt_t_min   0.181
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C67 \\sim F19A \\sim F20A \\sim F21A \\sim F19 \\sim F21 \\sim F20: within 1.7A
with sigma of 0.01 and sigma for terminal atoms of 0.04
C60 \\sim F16A \\sim F17A \\sim F18A \\sim F17 \\sim F16 \\sim F18: within 1.7A
with sigma of 0.01 and sigma for terminal atoms of 0.04
C68 \\sim F22A \\sim F23A \\sim F24A \\sim F23 \\sim F22 \\sim F24: within 1.7A
with sigma of 0.01 and sigma for terminal atoms of 0.04
C75 \\sim F25A \\sim F26A \\sim F27A \\sim F27 \\sim F25 \\sim F26: within 1.7A
with sigma of 0.01 and sigma for terminal atoms of 0.04
C76 \\sim F28 \\sim F29 \\sim F30 \\sim Cl1 \\sim Cl2 \\sim C77 \\sim F23 \\sim
F19 \\sim F27 \\sim F17 \\sim F21 \\sim F25 \\sim F29A \\sim F16 \\sim F18
\\sim F20 \\sim F22 \\sim F24 \\sim F26 \\sim F28A \\sim F30A: within 1.7A with
sigma of 0.01 and sigma for terminal atoms of 0.04
Uanis(Ir1) = Uanis(Ir1A)
3. Others
 Sof(F16A)=Sof(F17A)=Sof(F18A)=1-FVAR(1)
 Sof(F17)=Sof(F16)=Sof(F18)=FVAR(1)
 Sof(F29A)=Sof(F28A)=Sof(F30A)=1-FVAR(2)
 Sof(F28)=Sof(F29)=Sof(F30)=FVAR(2)
 Sof(F25A)=Sof(F26A)=Sof(F27A)=1-FVAR(3)
 Sof(F27)=Sof(F25)=Sof(F26)=FVAR(3)
 Sof(F22A)=Sof(F23A)=Sof(F24A)=1-FVAR(4)
 Sof(F23)=Sof(F22)=Sof(F24)=FVAR(4)
 Sof(F19A)=Sof(F20A)=Sof(F21A)=1-FVAR(5)
 Sof(F19)=Sof(F21)=Sof(F20)=FVAR(5)
 Sof(Ir1A)=1-FVAR(6)
 Sof(Ir1)=FVAR(6)
4.a Secondary CH2 refined with riding coordinates:
 C77(H77A,H77B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C11(H11), C12(H12), C13(H13), C14(H14), C17(H17),
 C18(H18), C19(H19), C20(H20), C22(H22), C24(H24), C25(H25), C29(H29), C30(H30),
  C32(H32), C33(H33), C46(H46), C48(H48), C50(H50), C54(H54), C56(H56),
 C58(H58), C62(H62), C64(H64), C66(H66), C70(H70), C72(H72), C74(H74)
4.c Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C34(H34A,H34B,H34C), C40(H40A,H40B,H40C), C41(H41A,H41B,
 H41C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C)
;
_shelx_res_checksum              70266
_shelx_hkl_checksum              34553
_shelx_shelxl_version_number     2014/7
_olex2_submission_original_sample_id 3CRT096
_olex2_submission_special_instructions 'No special instructions were received'