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_4087713
_publ_section_title
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 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         'C36 H46 B Co O P2'
_chemical_formula_sum            'C36 H46 B Co O P2'
_chemical_formula_weight         626.41
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-06-10
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 106.962(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.3070(7)
_cell_length_b                   8.9745(4)
_cell_length_c                   21.1421(9)
_cell_measurement_temperature    100
_cell_volume                     3322.5(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      99.99
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 VENTURE Kappa Duo PHOTON 100 CMOS'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0736
_diffrn_reflns_av_unetI/netI     0.0320
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            75454
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.541
_diffrn_reflns_theta_min         2.523
_exptl_absorpt_coefficient_mu    5.149
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_correction_T_min  0.5530
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1080 before and 0.0772 after correction.
The Ratio of minimum to maximum transmission is 0.7336.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_description       &#x0091;block&#x0092;
_exptl_crystal_F_000             1328
_refine_diff_density_max         0.499
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.049
_refine_ls_extinction_coef       0.00021(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         6791
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0392
_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^)+(0.0429P)^2^+2.4398P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0935
_refine_ls_wR_factor_ref         0.0980
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6021
_reflns_number_total             6791
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00530_si_002.cif
_cod_data_source_block           compound2a
_cod_database_code               4087713
_shelxl_version_number           2013-2
_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.a Ternary CH refined with riding coordinates:
 C16(H16), C25(H25), C13(H13), C28(H28)
2.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C11(H11), C6(H6), C10(H10), C20(H20), C2(H2), C32(H32),
 C23(H23), C36(H36), C21(H21), C35(H35), C5(H5), C3(H3), C4(H4), C22(H22),
 C34(H34), C33(H33)
2.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C17(H17A,H17B,H17C), C15(H15A,H15B,H15C), C30(H30A,H30B,
 H30C), C14(H14A,H14B,H14C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C29(H29A,
 H29B,H29C)
;
_olex2_submission_special_instructions 'No special instructions were received'