Cation-Modulated Reactivity of Iridium Hydride Pincer-Crown Ether Complexes.
Kita, Matthew R.; Miller, Alexander J. M.; Journal of the American Chemical Society 136 (2014) 14519–; doi:10.1021/ja507324s

data_4122733
_publ_section_title
;
 Cation-Modulated Reactivity of Iridium Hydride Pincer-Crown Ether
 Complexes.
;
_journal_issue                   41
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14519
_journal_paper_doi               10.1021/ja507324s
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         'C23 H39 Ir N O5 P, C32 H12 B F24'
_chemical_formula_sum            'C55 H51 B F24 Ir N O5 P'
_chemical_formula_weight         1495.95
_chemical_name_common            'Complex 2'
_chemical_name_systematic        block
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-07-08
_audit_creation_method
;
Olex2 1.2
(compiled 2014.06.27 svn.r2953 for OlexSys, GUI svn.r4855)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 98.0262(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   35.8564(5)
_cell_length_b                   12.8798(2)
_cell_length_c                   26.6812(3)
_cell_measurement_reflns_used    9920
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      70.15
_cell_measurement_theta_min      3.345
_cell_volume                     12201.3(3)
_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., 2013)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_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     1.54178
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_unetI/netI     0.0275
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            52433
_diffrn_reflns_theta_full        70.30
_diffrn_reflns_theta_max         70.30
_diffrn_reflns_theta_min         2.49
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.570
_exptl_absorpt_correction_T_max  0.8028
_exptl_absorpt_correction_T_min  0.5184
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0861 before and 0.0445 after correction.
The Ratio of minimum to maximum transmission is 0.6457.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.629
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5928
_exptl_crystal_preparation
'grown from toluene pentane slow vapor diffusion at -30C'
_exptl_crystal_recrystallization_method
'Crystals grown from slow vapor diffusion of toluene/pentane'
_exptl_crystal_size_max          0.359
_exptl_crystal_size_mid          0.252
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.225
_refine_diff_density_min         -0.881
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     825
_refine_ls_number_reflns         11437
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0287
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0405P)^2^+26.2018P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0728
_refine_ls_wR_factor_ref         0.0746
_reflns_number_gt                10342
_reflns_number_total             11437
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja507324s_si_003.cif
_cod_data_source_block           mk101
_cod_depositor_comments
'Adding full bibliography for 4122732--4122733.cif.'
_cod_database_code               4122733
_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(F8A) \\sim Ueq, Uanis(F8) \\sim Ueq, Uanis(F7A) \\sim Ueq, Uanis(F7)
\\sim Ueq, Uanis(F9A) \\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(C38) \\sim Ueq:
with sigma of 0.005 and sigma for terminal atoms of 0.005
3. Others
 Sof(F7)=Sof(F9)=Sof(F8)=1-FVAR(1)
 Sof(F7A)=Sof(F9A)=Sof(F8A)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C4(H4), C1(H1)
4.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C23(H23A,H23B), C14(H14A,H14B), C22(H22A,H22B), C15(H15A,
 H15B), C16(H16A,H16B), C20(H20A,H20B), C21(H21A,H21B), C19(H19A,H19B),
 C18(H18A,H18B), C17(H17A,H17B)
4.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C8(H8), C29(H29), C37(H37), C35(H35), C33(H33), C25(H25), C27(H27),
 C41(H41), C45(H45), C43(H43), C51(H51), C53(H53), C9(H9), C49(H49)
4.d Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C2(H2A,H2B,H2C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C)
;
_olex2_exptl_crystal_mounting_method
;Crystals mounted using polymer tips and
 paratone oil. Crystals mounted at 100K.
;
_olex2_submission_original_sample_id MK101
_olex2_submission_special_instructions 'No special instructions were received'