Diverse Cation-Promoted Reactivity of Iridium Carbonyl Pincer-Crown Ether Complexes
Grajeda, Javier; Kita, Matthew R.; Gregor, Lauren C.; White, Peter S.; Miller, Alexander J. M.; Organometallics 35 (2016) 306–316; doi:10.1021/acs.organomet.5b00786

data_4086401
_publ_contact_author_name
;
;
_publ_section_title
;
 Diverse Cation-Promoted Reactivity of Iridium Carbonyl Pincer-Crown Ether
 Complexes
;
_journal_name_full               Organometallics
_journal_page_first              306
_journal_page_last               316
_journal_paper_doi               10.1021/acs.organomet.5b00786
_journal_volume                  35
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C24 H40 Cl Ir N O6 P'
_chemical_formula_sum            'C24 H40 Cl Ir N O6 P'
_chemical_formula_weight         697.19
_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_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-05-11
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 91.0496(16)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.7702(5)
_cell_length_b                   11.7884(6)
_cell_length_c                   11.7937(6)
_cell_measurement_reflns_used    9975
_cell_measurement_temperature    100
_cell_measurement_theta_max      72.19
_cell_measurement_theta_min      3.75
_cell_volume                     1358.11(12)
_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 1.000
_diffrn_measured_fraction_theta_max 0.998
_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  0.0306
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            37886
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.184
_diffrn_reflns_theta_min         3.748
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    11.295
_exptl_absorpt_correction_T_max  0.4204
_exptl_absorpt_correction_T_min  0.1709
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0785 before and 0.0634 after correction.
The Ratio of minimum to maximum transmission is 0.4065.
The \l/2 correction factor is 0.00150.
;
_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    1.705
_exptl_crystal_description       block
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.213
_exptl_crystal_size_mid          0.158
_exptl_crystal_size_min          0.127
_refine_diff_density_max         1.641
_refine_diff_density_min         -0.899
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.040(9)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.157
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         5160
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.157
_refine_ls_R_factor_all          0.0181
_refine_ls_R_factor_gt           0.0181
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0256P)^2^+0.7117P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0473
_refine_ls_wR_factor_ref         0.0474
_reflns_Friedel_coverage         0.902
_reflns_friedel_fraction_full    1.000
_reflns_friedel_fraction_max     0.998
_reflns_number_gt                5142
_reflns_number_total             5160
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00786_si_002.cif
_cod_data_source_block           x1505003
_cod_depositor_comments
;Separating journal page numbers, which were accidentally combined
 together.
;
_cod_database_code               4086401
_shelx_estimated_absorpt_t_max   0.328
_shelx_estimated_absorpt_t_min   0.197
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.960(9) 0.040(9)
2. 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
3. Restrained distances
 Ir1-H
 1.9 with sigma of 0.005
4.a Ternary CH refined with riding coordinates:
 C6(H6), C9(H9)
4.b Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C21(H21A,H21B), C22(H22A,H22B), C24(H24A,H24B), C25(H25A,
 H25B), C27(H27A,H27B), C28(H28A,H28B), C30(H30A,H30B), C31(H31A,H31B),
 C33(H33A,H33B), C34(H34A,H34B)
4.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C16(H16)
4.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C)
;
_shelx_res_checksum              86017
_shelx_hkl_checksum              49626
_shelx_shelxl_version_number     2014/7
_olex2_submission_original_sample_id JG-I-201
_olex2_submission_special_instructions 'No special instructions were received'