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_4087711
_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         'C39 H49 B Fe N2 P2'
_chemical_formula_sum            'C39 H49 B Fe N2 P2'
_chemical_formula_weight         673.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                90
_cell_angle_beta                 102.923(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.9514(10)
_cell_length_b                   22.7818(15)
_cell_length_c                   13.2520(11)
_cell_measurement_temperature    100(2)
_cell_volume                     3516.8(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 1.000
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0794
_diffrn_reflns_av_unetI/netI     0.0892
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            115929
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         35.473
_diffrn_reflns_theta_min         1.788
_exptl_absorpt_coefficient_mu    0.544
_exptl_absorpt_correction_type   &#x0091;none&#x0092;
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_description       &#x0091;block&#x0092;
_exptl_crystal_F_000             1430
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.679
_refine_diff_density_min         -0.599
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         15227
_refine_ls_number_restraints     431
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.1020
_refine_ls_R_factor_gt           0.0457
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0528P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1012
_refine_ls_wR_factor_ref         0.1134
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9107
_reflns_number_total             15227
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00530_si_002.cif
_cod_data_source_block           compound1d
_cod_database_code               4087711
_shelxl_version_number           2013-2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All H(H) groups, All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C9-N1 \\sim C109-N101
 with sigma of 0.02
 C8-C9 \\sim C108-C109
 with sigma of 0.02
 C7-C8 \\sim C107-C108
 with sigma of 0.02
 C6-C7 \\sim C106-C107
 with sigma of 0.02
 C5-C6 \\sim C105-C106
 with sigma of 0.02
 C4-C5 \\sim C104-C105
 with sigma of 0.02
 C3-C4 \\sim C103-C104
 with sigma of 0.02
 C2-C3 \\sim C102-C103
 with sigma of 0.02
 C1-C2 \\sim C101-C102
 with sigma of 0.02
 N1-C1 \\sim N101-C101
 with sigma of 0.02
 N2-C2 \\sim N102-C102
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N102 \\sim C102 \\sim C103 \\sim C104 \\sim C105 \\sim C106 \\sim C101 \\sim
N101 \\sim C109 \\sim C108 \\sim C107: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
N102 \\sim N1 \\sim N101 \\sim N2 \\sim C109 \\sim C2 \\sim C101 \\sim C1 \\sim
C102 \\sim C9 \\sim C8 \\sim C103 \\sim C7 \\sim C104 \\sim C6 \\sim C105 \\sim
C106 \\sim C5 \\sim C4 \\sim C107 \\sim C3 \\sim C108: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 C101, C102, N102, C103, C104, C105, C106, C107, C108, C109, N101
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(N102)=Sof(N101)=Sof(C102)=Sof(C106)=Sof(C105)=Sof(H105)=Sof(C101)=
 Sof(C108)=Sof(H108)=Sof(C104)=Sof(H104)=Sof(C103)=Sof(H103)=Sof(C107)=
 Sof(H107)=Sof(C109)=Sof(H109)=Sof(Fe1A)=Sof(H102)=1-FVAR(1)
 Sof(Fe1)=Sof(N1)=Sof(C1)=Sof(N2)=Sof(C2)=Sof(C4)=Sof(H4)=Sof(C8)=Sof(H8)=
 Sof(C3)=Sof(H3)=Sof(C6)=Sof(C9)=Sof(H9)=Sof(C5)=Sof(H5)=Sof(C7)=Sof(H7)=
 Sof(H2)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C31(H31), C19(H19), C28(H28), C16(H16)
6.b Aromatic/amide H refined with riding coordinates:
 C26(H26), C38(H38), C12(H12), C24(H24), C35(H35), C23(H23), C4(H4), C8(H8),
 C3(H3), C13(H13), C15(H15), C14(H14), C39(H39), C37(H37), C25(H25), C9(H9),
 C5(H5), C36(H36), C7(H7), C105(H105), C108(H108), C104(H104), C103(H103),
 C107(H107), C109(H109)
6.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C33(H33A,H33B,H33C), C30(H30A,H30B,H30C), C32(H32A,H32B,
 H32C), C18(H18A,H18B,H18C), C29(H29A,H29B,H29C), C20(H20A,H20B,H20C), C17(H17A,
 H17B,H17C)
;
_olex2_submission_special_instructions 'No special instructions were received'