Hydrogenolysis of Tantalum Hydrocarbyl Complexes: Intermediates on the Road to a Dinuclear Tantalum Tetrahydride Derivative
Parker, Kyle D. J.; Nied, Dominik; Fryzuk, Michael D.; Organometallics 34 (2015) 3546–; doi:10.1021/acs.organomet.5b00344

data_4087584
_publ_section_title
;
 Hydrogenolysis of Tantalum Hydrocarbyl Complexes: Intermediates on the
 Road to a Dinuclear Tantalum Tetrahydride Derivative
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3546
_journal_paper_doi               10.1021/acs.organomet.5b00344
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C51 H56 N2 P Ta, C6 H6'
_chemical_formula_sum            'C57 H62 N2 P Ta'
_chemical_formula_weight         987.00
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-04-22
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                82.5839(8)
_cell_angle_beta                 89.1893(8)
_cell_angle_gamma                77.0839(8)
_cell_formula_units_Z            2
_cell_length_a                   11.4235(2)
_cell_length_b                   12.6093(2)
_cell_length_c                   18.0686(3)
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.95
_cell_measurement_theta_min      1.67
_cell_volume                     2515.28(7)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Burla et al., 2007)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0332
_diffrn_reflns_av_unetI/netI     0.0341
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            31085
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        24.950
_diffrn_reflns_theta_max         24.950
_diffrn_reflns_theta_min         1.671
_exptl_absorpt_coefficient_mu    2.254
_exptl_absorpt_correction_T_max  0.5701
_exptl_absorpt_correction_T_min  0.4231
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_description       prism
_exptl_crystal_F_000             1012
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.777
_refine_diff_density_min         -1.806
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     746
_refine_ls_number_reflns         8690
_refine_ls_number_restraints     835
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0424
_refine_ls_R_factor_gt           0.0310
_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^)+(0.0148P)^2^+4.3834P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0632
_refine_ls_wR_factor_ref         0.0672
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7433
_reflns_number_total             8690
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00344_si_002.cif
_cod_data_source_block           mf868_0m
_cod_original_cell_volume        2515.26(11)
_cod_database_code               4087584
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C20-C15 \\sim C20A-C15A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C14) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C17)
\\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C20) \\sim Ueq,
Uanis(C21) \\sim Ueq, Uanis(C22) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(P01A) = Uanis(P01)
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C46)=Sof(C47)=Sof(H47)=Sof(C48)=Sof(H48)=Sof(C49)=Sof(H49)=Sof(C50)=
 Sof(H50)=Sof(C51)=Sof(H51)=1-FVAR(1)
 Sof(C46B)=Sof(C47B)=Sof(H47B)=Sof(C48B)=Sof(H48B)=Sof(C49B)=Sof(H49B)=
 Sof(C50B)=Sof(H50B)=Sof(C51B)=Sof(H51B)=FVAR(1)
 Sof(P01A)=Sof(N02A)=Sof(C07A)=Sof(C08A)=Sof(H08A)=Sof(C09A)=Sof(C10A)=
 Sof(H10A)=Sof(C11A)=Sof(H11A)=Sof(C12A)=Sof(C13A)=Sof(H13D)=Sof(H13E)=
 Sof(H13F)=Sof(C14A)=Sof(C15A)=Sof(C16A)=Sof(H16A)=Sof(C17A)=Sof(C18A)=
 Sof(H18A)=Sof(C19A)=Sof(C20A)=Sof(H20D)=Sof(H20E)=Sof(H20F)=Sof(C21A)=
 Sof(H21D)=Sof(H21E)=Sof(H21F)=Sof(C22A)=Sof(H22D)=Sof(H22E)=Sof(H22F)=1-FVAR(2)
 Sof(P01)=Sof(N02)=Sof(C07)=Sof(C08)=Sof(H08)=Sof(C09)=Sof(C10)=Sof(H10)=
 Sof(C11)=Sof(H11)=Sof(C12)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C14)=
 Sof(C15)=Sof(C16)=Sof(H16)=Sof(C17)=Sof(C18)=Sof(H18)=Sof(C19)=Sof(C20)=
 Sof(H20A)=Sof(H20B)=Sof(H20C)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=Sof(C22)=
 Sof(H22A)=Sof(H22B)=Sof(H22C)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C40(H40A,H40B), C43(H43A,H43B), C45(H45A,H45B)
6.b Me refined with riding coordinates:
 C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C38(H38A,H38B,
 H38C), C39(H39A,H39B,H39C), C44(H44A,H44B,H44C)
6.c Aromatic/amide H refined with riding coordinates:
 C02(H02), C03(H03), C04(H04), C05(H05), C06(H06), C25(H25), C27(H27),
 C33(H33), C34(H34), C36(H36), C08(H08), C10(H10), C11(H11), C16(H16), C18(H18),
  C47(H47), C48(H48), C49(H49), C50(H50), C51(H51), C08A(H08A), C10A(H10A),
 C11A(H11A), C16A(H16A), C18A(H18A), C47B(H47B), C48B(H48B), C49B(H49B),
 C50B(H50B), C51B(H51B), C0AA(H0AA), C1AA(H1AA), C2(H2), C2AA(H2AA), C5(H5),
 C6(H6)
6.d Fitted hexagon refined as free rotating group:
 C46(C47,C48,C49,C50,C51), C46B(C47B,C48B,C49B,C50B,C51B)
6.e Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C13A(H13D,H13E,H13F), C20A(H20D,H20E,H20F), C21A(H21D,H21E,H21F),
 C22A(H22D,H22E,H22F)
;
_shelx_res_checksum              77702
_shelx_hkl_checksum              94952
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'