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_4086875
_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         'C27 H28 Ir, C32 H12 B F25.48'
_chemical_formula_sum            'C59 H40 B F25.41 Ir'
_chemical_formula_weight         1434.80
_chemical_name_systematic
'1,5-cyclooctadiene-n6-triphenylmethane iridium(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             2015-10-20
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                73.679(6)
_cell_angle_beta                 69.073(6)
_cell_angle_gamma                74.540(6)
_cell_formula_units_Z            2
_cell_length_a                   12.6001(14)
_cell_length_b                   13.9638(15)
_cell_length_c                   17.4035(18)
_cell_measurement_reflns_used    9986
_cell_measurement_temperature    90
_cell_measurement_theta_max      61.034
_cell_measurement_theta_min      4.943
_cell_volume                     2697.2(5)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      90
_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  0.0287
_diffrn_reflns_av_unetI/netI     0.0284
_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       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            63474
_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         30.694
_diffrn_reflns_theta_min         1.280
_exptl_absorpt_coefficient_mu    2.604
_exptl_absorpt_correction_T_max  0.7911
_exptl_absorpt_correction_T_min  0.6605
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0671 before and 0.0366 after correction.
The Ratio of minimum to maximum transmission is 0.8350.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.767
_exptl_crystal_description       prism
_exptl_crystal_F_000             1409
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.372
_refine_diff_density_min         -1.443
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     831
_refine_ls_number_reflns         16610
_refine_ls_number_restraints     1125
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0315
_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^)+(0.0463P)^2^+4.3589P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0832
_refine_ls_wR_factor_ref         0.0857
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15148
_reflns_number_total             16610
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00784_si_002.cif
_cod_data_source_block           Complex_[18][BArF4]
_cod_database_code               4086875
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C43-F00M \\sim C43-F00H \\sim C43-F00K \\sim C43-F7AA \\sim C43-F3AA \\sim
C43-F6AA \\sim C43-F4AA ~
 C43-F5AA \\sim C43-F00N
 with sigma of 0.02
 F00M-F00H \\sim F00H-F00K \\sim F00K-F00M \\sim F7AA-F3AA \\sim F3AA-F6AA
\\sim F6AA-F7AA \\sim F4AA-
 F5AA \\sim F5AA-F00N \\sim F00N-F4AA
 with sigma of 0.02
 C34-F11 \\sim C34-F12 \\sim C34-F10 \\sim C34-F11A \\sim C34-F12A \\sim
C34-F10A \\sim C34-F2AA \\sim C34-
 F0AA \\sim C34-F1AA
 with sigma of 0.02
 F11-F12 \\sim F12-F10 \\sim F10-F11 \\sim F11A-F12A \\sim F12A-F10A \\sim
F10A-F11A \\sim F2AA-F0AA ~
 F0AA-F1AA \\sim F1AA-F2AA
 with sigma of 0.02
 C35-F3 \\sim C35-F8AA \\sim C35-F1 \\sim C35-F1A \\sim C35-F4A \\sim C35-F2
 with sigma of 0.02
 F3-F8AA \\sim F8AA-F1 \\sim F1-F3 \\sim F1A-F4A \\sim F4A-F2 \\sim F2-F1A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F12) = Uanis(F12A)
Uanis(F10) = Uanis(F10A)
Uanis(F11) = Uanis(F11A)
Uanis(F12) = Uanis(F0AA)
Uanis(F10) = Uanis(F1AA)
Uanis(F11) = Uanis(F2AA)
Uanis(F00H) = Uanis(F3AA)
Uanis(F00H) = Uanis(F4AA)
Uanis(F00K) = Uanis(F5AA)
Uanis(F00K) = Uanis(F6AA)
Uanis(F00M) = Uanis(F00N)
Uanis(F00M) = Uanis(F7AA)
Uanis(F1) = Uanis(F1A)
Uanis(F4A) = Uanis(F8AA)
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(F0AA)=1-FVAR(1)
 Sof(F12)=FVAR(1)
 Sof(F1AA)=1-FVAR(2)
 Sof(F10)=FVAR(2)
 Sof(F2AA)=1-FVAR(3)
 Sof(F11)=FVAR(3)
 Sof(F4AA)=1-FVAR(4)
 Sof(F00H)=FVAR(4)
 Sof(F6AA)=1-FVAR(5)
 Sof(F00K)=FVAR(5)
 Sof(F7AA)=1-FVAR(6)
 Sof(F00M)=FVAR(6)
 Sof(F1A)=1-FVAR(7)
 Sof(F1)=FVAR(7)
 Sof(F8AA)=1-FVAR(8)
 Sof(F4A)=FVAR(8)
6.a Ternary CH refined with riding coordinates:
 C21(H21), C25(H25), C7(H7), C24(H24), C20(H20)
6.b Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C23(H23A,H23B), C22(H22A,H22B), C26(H26A,H26B)
6.c Aromatic/amide H refined with riding coordinates:
 C41(H41), C56(H56), C48(H48), C29(H29), C52(H52), C46(H46), C13(H13),
 C012(H012), C39(H39), C33(H33), C37(H37), C54(H54), C31(H31), C2(H2), C3(H3),
 C12(H12), C10(H10), C6(H6), C15(H15), C11(H11), C1(H1), C5(H5), C9(H9),
 C16(H16), C17(H17), C19(H19), C18(H18)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'