Accessing δ-B‒H Coordinated Complexes of Rh(I) and Ir(I) Using Mono- and Dihydroboranes: Cooperative Stabilization by a Phosphoramidate Coligand
Drover, Marcus W.; Bowes, Eric G.; Love, Jennifer A.; Schafer, Laurel L.; Organometallics  (2016) –; doi:10.1021/acs.organomet.6b00784

data_4086876
_publ_section_title
;
 Accessing \d-B--H Coordinated Complexes of Rh(I) and Ir(I) Using Mono-
 and Dihydroboranes: Cooperative Stabilization by a Phosphoramidate
 Coligand
;
_journal_name_full               Organometallics
_journal_paper_doi               10.1021/acs.organomet.6b00784
_journal_year                    2016
_chemical_formula_moiety         'C32 H12 B F24, C16 H23 Ir N'
_chemical_formula_sum            'C47.96 H35 B F24 Ir N'
_chemical_formula_weight         1284.30
_chemical_name_systematic
'n6-triphenylmethane-1,5-cyclooctadieneiridium(I) tetrakis(3,5-trifluoromethylphenyl)borate'
_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
_audit_creation_date             2016-09-28
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_cell_angle_alpha                100.771(4)
_cell_angle_beta                 101.143(4)
_cell_angle_gamma                119.129(3)
_cell_formula_units_Z            2
_cell_length_a                   13.039(2)
_cell_length_b                   13.042(2)
_cell_length_c                   17.176(3)
_cell_measurement_reflns_used    9695
_cell_measurement_temperature    90
_cell_measurement_theta_max      30.553
_cell_measurement_theta_min      2.632
_cell_volume                     2365.0(7)
_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      90.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker Apex Duo II'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_av_unetI/netI     0.0346
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            53815
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.604
_diffrn_reflns_theta_min         1.279
_exptl_absorpt_coefficient_mu    2.954
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5061
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0994 before and 0.0480 after correction.
The Ratio of minimum to maximum transmission is 0.6783.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.804
_exptl_crystal_description       prism
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.13
_refine_diff_density_max         2.382
_refine_diff_density_min         -3.304
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     690
_refine_ls_number_reflns         14467
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0380
_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^)+(0.0565P)^2^+4.8779P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0960
_refine_ls_wR_factor_ref         0.1005
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13070
_reflns_number_total             14467
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00784_si_002.cif
_cod_data_source_block           Complex_[20][BArF4]
_cod_database_code               4086876
_shelx_estimated_absorpt_t_max   0.700
_shelx_estimated_absorpt_t_min   0.392
_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(F23) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.02
Uanis(F11) = Uanis(F11A)
Uanis(F12) = Uanis(F12A)
Uanis(F10) = Uanis(F10A)
3. Others
 Sof(F11A)=1-FVAR(1)
 Sof(F11)=FVAR(1)
 Sof(F12A)=1-FVAR(2)
 Sof(F12)=FVAR(2)
 Sof(F10A)=1-FVAR(3)
 Sof(F10)=FVAR(3)
4.a Ternary CH refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C13(H13), C14(H14)
4.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B), C15(H15A,H15B), C16(H16A,H16B)
4.c Aromatic/amide H refined with riding coordinates:
 C18(H18), C20(H20), C22(H22), C26(H26), C28(H28), C30(H30), C34(H34),
 C36(H36), C38(H38), C42(H42), C44(H44), C46(H46)
4.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'