E‒H Bond Activations and Hydrosilylation Catalysis with Iron and Cobalt Metalloboranes
Nesbit, Mark A.; Suess, Daniel L. M.; Peters, Jonas C.; Organometallics 34 (2015) 4741–; doi:10.1021/acs.organomet.5b00530

data_4087712
_publ_section_title
;
 E--H Bond Activations and Hydrosilylation Catalysis with Iron and Cobalt
 Metalloboranes
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              4741
_journal_paper_doi               10.1021/acs.organomet.5b00530
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety
'0.17(C60 H82 B2 Co2 N2 P4), 0.67(C30 H41 B Co N2 P2)'
_chemical_formula_sum            'C30 H41 B Co N1.67 P2'
_chemical_formula_weight         556.66
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-06-11
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                69.741(5)
_cell_angle_beta                 81.149(4)
_cell_angle_gamma                74.584(3)
_cell_formula_units_Z            6
_cell_length_a                   10.7517(7)
_cell_length_b                   18.0184(12)
_cell_length_c                   24.6119(15)
_cell_measurement_reflns_used    9425
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.21
_cell_measurement_theta_min      2.21
_cell_volume                     4302.0(5)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.910
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1027
_diffrn_reflns_av_unetI/netI     0.1333
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.910
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            206530
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.910
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         33.129
_diffrn_reflns_theta_min         1.736
_exptl_absorpt_coefficient_mu    0.731
_exptl_absorpt_correction_type   &#x0091;none&#x0092;
_exptl_crystal_colour            &#x0091;red&#x0092;
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_description       &#x0091;block&#x0092;
_exptl_crystal_F_000             1768
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.856
_refine_diff_density_min         -0.660
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1029
_refine_ls_number_reflns         29815
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.1205
_refine_ls_R_factor_gt           0.0536
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0665P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1356
_refine_ls_wR_factor_ref         0.1512
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16184
_reflns_number_total             29815
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00530_si_002.cif
_cod_data_source_block           compound2
_cod_database_code               4087712
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.944
_shelx_estimated_absorpt_t_min   0.827
_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
C8B \\sim C8A \\sim C7B \\sim C7A \\sim C9B \\sim C9A: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
3. Rigid body (RIGU) restrains
 C8B, C8A, C7B, C7A, C9B, C9A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C9B)=Sof(H9BA)=Sof(H9BB)=Sof(H9BC)=Sof(C7B)=Sof(H7B)=Sof(C8B)=Sof(H8BA)=
 Sof(H8BB)=Sof(H8BC)=1-FVAR(1)
 Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=Sof(C7A)=Sof(H7A)=Sof(C9A)=Sof(H9AA)=
 Sof(H9AB)=Sof(H9AC)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C107(H107), C122(H122), C219(H219), C110(H110), C119(H119), C22(H22),
 C210(H210), C19(H19), C207(H207), C10(H10), C7B(H7B), C7A(H7A)
5.b Aromatic/amide H refined with riding coordinates:
 C203(H203), C126(H126), C106(H106), C15(H15), C226(H226), C130(H130),
 C227(H227), C103(H103), C117(H117), C115(H115), C228(H228), C205(H205),
 C129(H129), C230(H230), C118(H118), C105(H105), C204(H204), C104(H104),
 C17(H17), C229(H229), C3(H3), C18(H18), C27(H27), C127(H127), C215(H215),
 C128(H128), C218(H218), C16(H16), C5(H5), C116(H116), C217(H217), C216(H216),
 C30(H30), C6(H6), C4(H4), C206(H206), C28(H28), C26(H26), C29(H29)
5.c Idealised Me refined as rotating group:
 C121(H12D,H12E,H12F), C124(H12G,H12H,H12I), C24(H24A,H24B,H24C), C112(H11D,
 H11E,H11F), C212(H21D,H21E,H21F), C123(H12J,H12K,H12L), C21(H21A,H21B,H21C),
 C111(H11G,H11H,H11I), C109(H10A,H10B,H10C), C23(H23A,H23B,H23C), C120(H12M,
 H12N,H12O), C224(H22A,H22B,H22C), C20(H20A,H20B,H20C), C108(H10D,H10E,H10F),
 C221(H22G,H22H,H22I), C209(H20D,H20E,H20F), C220(H22J,H22K,H22L), C12(H12A,
 H12B,H12C), C211(H21G,H21H,H21I), C208(H20G,H20H,H20I), C11(H11A,H11B,H11C),
 C9B(H9BA,H9BB,H9BC), C8A(H8AA,H8AB,H8AC), C8B(H8BA,H8BB,H8BC), C9A(H9AA,H9AB,
 H9AC)
;
_olex2_submission_special_instructions 'No special instructions were received'