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_4122732
_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 Cl Ir N O5 P'
_chemical_formula_sum            'C23 H39 Cl Ir N O5 P'
_chemical_formula_weight         668.17
_chemical_name_common            'Complex 1'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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                93.522(2)
_cell_angle_beta                 113.425(2)
_cell_angle_gamma                94.009(2)
_cell_formula_units_Z            2
_cell_length_a                   10.5376(4)
_cell_length_b                   11.9462(5)
_cell_length_c                   12.0486(5)
_cell_measurement_reflns_used    9155
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.66
_cell_measurement_theta_min      3.73
_cell_volume                     1381.71(10)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_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  0.0282
_diffrn_reflns_av_unetI/netI     0.0341
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7801
_diffrn_reflns_theta_full        66.74
_diffrn_reflns_theta_max         66.74
_diffrn_reflns_theta_min         3.73
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    11.045
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.0700
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1141 before and 0.0346 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.1495 before and 0.0663 after correction.
 The Ratio of minimum to maximum transmission is 0.42.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 32591 reflections, Rint = 0.0438
 (25910 with I > 3sig(I), Rint = 0.0411)
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.606
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             666
_exptl_crystal_preparation       'Complex 1 was prepared as described in SI.'
_exptl_crystal_recrystallization_method
'Single crystals of 1 were grown by pentane/toluene vapor diffusion at -30C.'
_exptl_crystal_size_max          0.514
_exptl_crystal_size_mid          0.151
_exptl_crystal_size_min          0.148
_refine_diff_density_max         1.456
_refine_diff_density_min         -1.194
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         4770
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0344
_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/[\s^2^(Fo^2^)+(0.0341P)^2^+8.6113P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0830
_refine_ls_wR_factor_ref         0.0858
_reflns_number_gt                4498
_reflns_number_total             4770
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja507324s_si_003.cif
_cod_data_source_block           x1303006
_cod_depositor_comments
'Adding full bibliography for 4122732--4122733.cif.'
_cod_original_cell_volume        1381.70(10)
_cod_database_code               4122732
_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.a Ternary CH refined with riding coordinates:
 C4(H4), C1(H1)
2.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C23(H23A,H23B), C14(H14A,H14B), C16(H16A,H16B), C22(H22A,
 H22B), C15(H15A,H15B), C17(H17A,H17B), C19(H19A,H19B), C20(H20A,H20B),
 C18(H18A,H18B), C21(H21A,H21B)
2.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C9(H9), C8(H8)
2.d Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C6(H6A,H6B,H6C), C5(H5A,H5B,H5C)
;
_olex2_submission_special_instructions 'No special instructions were received'