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_4087715
_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         'C43 H50 B Co N P2'
_chemical_formula_sum            'C43 H50 B Co N P2'
_chemical_formula_weight         712.52
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-06-15
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.5888(9)
_cell_length_b                   11.1243(7)
_cell_length_c                   16.8762(9)
_cell_measurement_temperature    100(2)
_cell_volume                     3677.5(3)
_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      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker KAPPA APEX II ccd'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1355
_diffrn_reflns_av_unetI/netI     0.1593
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            72653
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         36.433
_diffrn_reflns_theta_min         1.831
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.585
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.6846
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0760 before and 0.0715 after correction.
The Ratio of minimum to maximum transmission is 0.9163.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            &#x0091;orange&#x0092;
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_description       &#x0091;plate&#x0092;
_exptl_crystal_F_000             1508
_refine_diff_density_max         0.532
_refine_diff_density_min         -0.523
_refine_diff_density_rms         0.103
_refine_ls_abs_structure_details
;
 Flack x determined using 3699 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.021(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.976
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     445
_refine_ls_number_reflns         17585
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.976
_refine_ls_R_factor_all          0.1362
_refine_ls_R_factor_gt           0.0599
_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^)+(0.0256P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0898
_refine_ls_wR_factor_ref         0.1090
_reflns_Friedel_coverage         0.912
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.960
_reflns_number_gt                10448
_reflns_number_total             17585
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00530_si_002.cif
_cod_data_source_block           compound2c
_cod_database_code               4087715
_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:
 C29(H29), C26(H26), C38(H38), C41(H41)
2.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C12(H12), C5(H5), C13(H13), C21(H21), C24(H24), C9(H9), C11(H11),
 C6(H6), C19(H19), C4(H4), C34(H34), C36(H36), C22(H22), C23(H23), C33(H33),
 C8(H8), C18(H18), C35(H35), C16(H16), C17(H17)
2.c Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C42(H42A,H42B,H42C), C31(H31A,H31B,H31C), C27(H27A,H27B,
 H27C), C28(H28A,H28B,H28C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C43(H43A,
 H43B,H43C)
;
_olex2_submission_special_instructions 'No special instructions were received'