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_4087586
_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         'C76 H78 N4 P2 Ta2'
_chemical_formula_sum            'C76 H78 N4 O0 P2 Ta2'
_chemical_formula_weight         1471.26
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-04-15
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 90.320(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            4
_cell_length_a                   16.309(5)
_cell_length_b                   32.774(5)
_cell_length_c                   14.072(5)
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.74
_cell_measurement_theta_min      1.91
_cell_volume                     7522(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_unetI/netI     0.0562
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5046
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        22.745
_diffrn_reflns_theta_max         22.745
_diffrn_reflns_theta_min         1.907
_exptl_absorpt_coefficient_mu    2.990
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_description       plate
_exptl_crystal_F_000             2952
_refine_diff_density_max         1.584
_refine_diff_density_min         -0.852
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.745
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     333
_refine_ls_number_reflns         5046
_refine_ls_number_restraints     384
_refine_ls_restrained_S_all      0.729
_refine_ls_R_factor_all          0.0797
_refine_ls_R_factor_gt           0.0467
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1107P)^2^+72.6739P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1231
_refine_ls_wR_factor_ref         0.1415
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3341
_reflns_number_total             5046
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00344_si_002.cif
_cod_data_source_block           mf895_0m
_cod_database_code               4087586
_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. Restrained distances
 C1-C2 \\sim C17-C18
 with sigma of 0.04
 C1-C6 \\sim C17-C22
 with sigma of 0.04
 C2-C3 \\sim C18-C19
 with sigma of 0.04
 C5-C6 \\sim C21-C22
 with sigma of 0.04
 C3-C4 \\sim C19-C20
 with sigma of 0.04
 C4-C5 \\sim C20-C21
 with sigma of 0.04
 C2-C7 \\sim C18-C23
 with sigma of 0.04
 C4-C8 \\sim C20-C24
 with sigma of 0.04
 C6-C9 \\sim C22-C25
 with sigma of 0.04
3. Restrained planarity
 C17, C18, C22, C19, C21, C20, C25, C23, C24
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C1) = Uanis(C17)
Uanis(C6) = Uanis(C22)
Uanis(C5) = Uanis(C21)
Uanis(C4) = Uanis(C20)
Uanis(C3) = Uanis(C19)
Uanis(C2) = Uanis(C18)
Uanis(C9) = Uanis(C25)
Uanis(C8) = Uanis(C24)
Uanis(C7) = Uanis(C23)
5. 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
6.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C11(H11), C12(H12), C14(H14), C19(H19), C21(H21), C27(H27),
 C28(H28), C30(H30), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38)
6.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C16(H16A,H16B,H16C),
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C32(H32A,H32B,
 H32C)
;
_shelx_res_checksum              17631
_shelx_hkl_checksum              22362
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'