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_4087709
_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         'C36 H47 B Fe P2 S'
_chemical_formula_sum            'C36 H47 B Fe P2 S'
_chemical_formula_weight         640.39
_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                 110.525(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5444(9)
_cell_length_b                   19.5804(15)
_cell_length_c                   16.0331(13)
_cell_measurement_reflns_used    9982
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.72
_cell_measurement_theta_min      2.48
_cell_volume                     3394.1(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      99.99
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0877
_diffrn_reflns_av_unetI/netI     0.0558
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            115232
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         32.349
_diffrn_reflns_theta_min         1.709
_exptl_absorpt_coefficient_mu    0.624
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.6873
_exptl_absorpt_correction_type   &#x0091;multi-scan&#x0092;
_exptl_crystal_colour            &#x0091;orange&#x0092;
_exptl_crystal_density_diffrn    1.253
_exptl_crystal_description       &#x0091;block&#x0092;
_exptl_crystal_F_000             1360
_refine_diff_density_max         1.341
_refine_diff_density_min         -0.420
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     381
_refine_ls_number_reflns         11573
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0810
_refine_ls_R_factor_gt           0.0451
_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^)+(0.0451P)^2^+2.1301P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0961
_refine_ls_wR_factor_ref         0.1097
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8206
_reflns_number_total             11573
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00530_si_002.cif
_cod_data_source_block           compound1b
_cod_database_code               4087709
_shelxl_version_number           2013-2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 B1-H1
 1.12 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C16(H16), C13(H13), C31(H31), C34(H34)
3.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C2(H2), C4(H4), C5(H5), C3(H3), C11(H11), C20(H20), C26(H26),
 C10(H10), C21(H21), C8(H8), C23(H23), C24(H24), C27(H27), C9(H9), C29(H29),
 C28(H28), C22(H22)
3.c Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C18(H18A,H18B,H18C), C17(H17A,H17B,H17C), C33(H33A,H33B,
 H33C), C15(H15A,H15B,H15C), C14(H14A,H14B,H14C), C35(H35A,H35B,H35C), C36(H36A,
 H36B,H36C)
;
_olex2_submission_special_instructions 'No special instructions were received'