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_4086402
_publ_contact_author_name
;
;
_publ_section_title
;
 Diverse Cation-Promoted Reactivity of Iridium Carbonyl Pincer-Crown Ether
 Complexes
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_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_formula_moiety         'C24 H39 Ir N O6 P'
_chemical_formula_sum            'C24 H39 Ir N O6 P'
_chemical_formula_weight         660.73
_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     iterative
_audit_creation_date             2015-07-01
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                96.312(2)
_cell_angle_beta                 98.081(2)
_cell_angle_gamma                101.330(2)
_cell_formula_units_Z            4
_cell_length_a                   11.8015(3)
_cell_length_b                   13.5970(4)
_cell_length_c                   17.1601(5)
_cell_measurement_reflns_used    9945
_cell_measurement_temperature    100
_cell_measurement_theta_max      66.58
_cell_measurement_theta_min      2.63
_cell_volume                     2646.15(13)
_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 0.965
_diffrn_measured_fraction_theta_max 0.965
_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  0.0621
_diffrn_reflns_av_unetI/netI     0.0587
_diffrn_reflns_laue_measured_fraction_full 0.965
_diffrn_reflns_laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            29168
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        66.636
_diffrn_reflns_theta_max         66.636
_diffrn_reflns_theta_min         2.627
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.651
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.3352
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0806 before and 0.0548 after correction.
The Ratio of minimum to maximum transmission is 0.3352.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.659
_exptl_crystal_description       plate
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.142
_exptl_crystal_size_mid          0.106
_exptl_crystal_size_min          0.069
_refine_diff_density_max         3.165
_refine_diff_density_min         -0.787
_refine_diff_density_rms         0.204
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     603
_refine_ls_number_reflns         9023
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0665
_refine_ls_R_factor_gt           0.0482
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0734P)^2^+3.1797P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1161
_refine_ls_wR_factor_ref         0.1276
_reflns_Friedel_coverage         0.000
_reflns_friedel_fraction_full    .
_reflns_friedel_fraction_max     .
_reflns_number_gt                6967
_reflns_number_total             9023
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00786_si_002.cif
_cod_data_source_block           x1506013
_cod_depositor_comments
;Separating journal page numbers, which were accidentally combined
 together.
;
_cod_original_cell_volume        2646.16(13)
_cod_database_code               4086402
_shelx_estimated_absorpt_t_max   0.527
_shelx_estimated_absorpt_t_min   0.313
_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:
 C5(H5), C8(H8), C45(H45), C48(H48)
2.b Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C20(H20A,H20B), C21(H21A,H21B), C23(H23A,H23B), C24(H24A,
 H24B), C26(H26A,H26B), C27(H27A,H27B), C29(H29A,H29B), C30(H30A,H30B),
 C32(H32A,H32B), C33(H33A,H33B), C58(H58A,H58B), C60(H60A,H60B), C61(H61A,H61B),
  C63(H63A,H63B), C64(H64A,H64B), C66(H66A,H66B), C67(H67A,H67B), C69(H69A,
 H69B), C70(H70A,H70B), C72(H72A,H72B), C73(H73A,H73B)
2.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C15(H15), C53(H53), C54(H54), C55(H55)
2.d Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C),
 C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C49(H49A,H49B,H49C), C50(H50A,H50B,
 H50C)
;
_shelx_res_checksum              45670
_shelx_hkl_checksum              24425
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'