Toward anti-Markovnikov 1-Alkyne O-Phosphoramidation: Exploiting Metal-Ligand Cooperativity in a 1,3-N,O-Chelated Cp*Ir(III) Complex.
Drover, Marcus W.; Love, Jennifer A.; Schafer, Laurel L.; Journal of the American Chemical Society 138 (2016) 8396–8399; doi:10.1021/jacs.6b05143

data_4130613
_publ_section_title
;
 Toward anti-Markovnikov 1-Alkyne O-Phosphoramidation: Exploiting
 Metal-Ligand Cooperativity in a 1,3-N,O-Chelated Cp*Ir(III) Complex.
;
_journal_issue                   27
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8396
_journal_page_last               8399
_journal_paper_doi               10.1021/jacs.6b05143
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C32 H12 B F24, C28 H44 Ir N O3 P'
_chemical_formula_sum            'C60 H56 B F24 Ir N O3 P'
_chemical_formula_weight         1529.03
_chemical_name_systematic        'iridium vinyloxy'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-03-24
_audit_creation_method
;
Olex2 1.2
(compiled Feb 16 2016 13:09:46 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                110.651(2)
_cell_angle_beta                 95.629(2)
_cell_angle_gamma                97.244(2)
_cell_formula_units_Z            4
_cell_length_a                   14.0248(12)
_cell_length_b                   19.7867(17)
_cell_length_c                   24.657(2)
_cell_measurement_reflns_used    9971
_cell_measurement_temperature    90
_cell_measurement_theta_max      25.30
_cell_measurement_theta_min      2.287
_cell_volume                     6276.3(9)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      90.0
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker-Nonius APEXII CCD area detector'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device
'Bruker-Nonius APEXII CCD area detector and D8 diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0615
_diffrn_reflns_av_unetI/netI     0.0603
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            81329
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.370
_diffrn_reflns_theta_max         25.370
_diffrn_reflns_theta_min         0.893
_exptl_absorpt_coefficient_mu    2.268
_exptl_absorpt_correction_T_max  0.7792
_exptl_absorpt_correction_T_min  0.6216
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014) was used for absorption correction. wR2(int) was 0.0615 before and 0.0503 after correction. The Ratio of minimum to maximum transmission is 0.7976. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.618
_exptl_crystal_description       prism
_exptl_crystal_F_000             3040
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         3.016
_refine_diff_density_min         -1.308
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1715
_refine_ls_number_reflns         22905
_refine_ls_number_restraints     1656
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0695
_refine_ls_R_factor_gt           0.0397
_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^)+(0.0392P)^2^+8.3253P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0837
_refine_ls_wR_factor_ref         0.0956
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16907
_reflns_number_total             22905
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b05143_si_002.cif
_cod_data_source_block           finaljl217_a
_cod_original_cell_volume        6276.4(9)
_cod_database_code               4130613
_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
Uanis(C72) \\sim Ueq: with sigma of 0.0001 and sigma for terminal atoms of
0.0002
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(F5AB)=Sof(F4AB)=Sof(F3AB)=1-FVAR(1)
 Sof(F3AA)=Sof(F4AA)=Sof(F5AA)=FVAR(1)
 Sof(F6AB)=Sof(F7AB)=Sof(F8AB)=1-FVAR(2)
 Sof(F6AA)=Sof(F7AA)=Sof(F8AA)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C17(H17A,H17B), C19(H19A,H19B),
 C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C44(H44A,H44B), C46(H46A,H46B)
5.b Aromatic/amide H refined with riding coordinates:
 C89(H89), C91(H91), C93(H93), C97(H97), C99(H99), C101(H101), C105(H105),
 C107(H107), C109(H109), C113(H113), C115(H115), C117(H117), C57(H57), C59(H59),
  C61(H61), C65(H65), C67(H67), C69(H69), C73(H73), C75(H75), C77(H77),
 C81(H81), C83(H83), C85(H85), C2(H2), C23(H23), C24(H24), C25(H25), C29(H29),
 C50(H50), C51(H51), C52(H52)
5.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,
 H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C20(H20A,
 H20B,H20C), C27(H27A,H27B,H27C), C119(H11A,H11B,H11C), C33(H33A,H33B,H33C),
 C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,
 H42C), C43(H43A,H43B,H43C), C45(H45A,H45B,H45C), C47(H47A,H47B,H47C), C54(H54A,
 H54B,H54C), C55(H55A,H55B,H55C)
;
_shelx_res_checksum              38171
_shelx_hkl_checksum              69108
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'