Synthesis of a Tris(phosphaalkene)phosphine Ligand and Fundamental Organometallic Reactions on Its Sterically Shielded Metal Complexes
Miura-Akagi, Preston M.; Nakashige, Mika L.; Maile, Caitlin K.; Oshiro, Shelly M.; Gurr, Joshua R.; Yoshida, Wesley Y.; Royappa, A. Timothy; Krause, Colleen E.; Rheingold, Arnold L.; Hughes, Russell P.; Cain, Matthew F.; Organometallics 35 (2016) 2224–; doi:10.1021/acs.organomet.6b00250

data_4086584
_publ_contact_author_name
;
;
_publ_section_title
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 Synthesis of a Tris(phosphaalkene)phosphine Ligand and Fundamental
 Organometallic Reactions on Its Sterically Shielded Metal Complexes
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              2224
_journal_paper_doi               10.1021/acs.organomet.6b00250
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C75 H99 Cl1 Ir1 P4, C1 H1 Cl3'
_chemical_formula_sum            'C76 H100 Cl4 Ir P4'
_chemical_formula_weight         1471.43
_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_Hall           '-P 3'
_space_group_name_H-M_alt        'P -3'
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-02-19
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   18.6016(7)
_cell_length_b                   18.6016(7)
_cell_length_c                   14.2012(6)
_cell_measurement_reflns_used    9781
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.684
_cell_measurement_theta_min      2.190
_cell_volume                     4255.6(3)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.928
_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  0.0478
_diffrn_reflns_av_unetI/netI     0.0318
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.928
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            78720
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.928
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.115
_diffrn_reflns_theta_min         1.912
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.804
_exptl_absorpt_correction_T_max  0.0991
_exptl_absorpt_correction_T_min  0.0678
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0719 before and 0.0458 after correction.
The Ratio of minimum to maximum transmission is 0.6842.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.148
_exptl_crystal_description       plate
_exptl_crystal_F_000             1522
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.134
_refine_diff_density_min         -1.188
_refine_diff_density_rms         0.085
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         7770
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0327
_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^)+(0.0465P)^2^+2.6875P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0799
_refine_ls_wR_factor_ref         0.0847
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6582
_reflns_number_total             7770
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00250_si_003.cif
_cod_data_source_block           cain30_a_sq
_cod_original_cell_volume        4255.6(4)
_cod_database_code               4086584
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C21) = Uanis(C19')
Uanis(C20) = Uanis(C21')
Uanis(C19) = Uanis(C20')
3. Others
 Sof(C23')=Sof(H23D)=Sof(H23E)=Sof(H23F)=Sof(C24')=Sof(H24D)=Sof(H24E)=
 Sof(H24F)=Sof(C25')=Sof(H25D)=Sof(H25E)=Sof(H25F)=1-FVAR(1)
 Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=
 Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=FVAR(1)
 Sof(C19')=Sof(H19D)=Sof(H19E)=Sof(H19F)=Sof(C20')=Sof(H20D)=Sof(H20E)=
 Sof(H20F)=Sof(C21')=Sof(H21D)=Sof(H21E)=Sof(H21F)=1-FVAR(2)
 Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=
 Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=FVAR(2)
4.a Ternary CH refined with riding coordinates:
 C26(H26)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C10(H10), C12(H12)
4.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C19(H19A,H19B,
 H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C24(H24A,
 H24B,H24C), C25(H25A,H25B,H25C), C19'(H19D,H19E,H19F), C20'(H20D,H20E,H20F),
 C21'(H21D,H21E,H21F), C23'(H23D,H23E,H23F), C24'(H24D,H24E,H24F), C25'(H25D,
 H25E,H25F)
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_shelx_res_checksum              2605
_shelx_hkl_checksum              85751
_shelx_fab_checksum              85669
_shelx_shelxl_version_number     2014/7
_olex2_submission_original_sample_id 'MC 2-48A'
_olex2_submission_special_instructions 'No special instructions were received'