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_4087587
_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         'C53 H64 N2 P Si2 Ta, C4 H10 O'
_chemical_formula_sum            'C57 H74 N2 O P Si2 Ta'
_chemical_formula_weight         1071.28
_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   geom
_atom_sites_solution_primary     direct
_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
_cell_angle_beta                 92.1840(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1271(3)
_cell_length_b                   20.5083(6)
_cell_length_c                   21.0150(5)
_cell_measurement_reflns_used    9843
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.148
_cell_measurement_theta_min      2.208
_cell_volume                     5222.8(2)
_computing_cell_refinement       'SAINT v7.60A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.60A (Bruker, 2009)'
_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      173.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            45376
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.148
_diffrn_reflns_theta_min         1.908
_exptl_absorpt_coefficient_mu    2.221
_exptl_absorpt_correction_T_max  0.7166
_exptl_absorpt_correction_T_min  0.6092
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_description       plate
_exptl_crystal_F_000             2216
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.664
_refine_diff_density_min         -0.565
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     588
_refine_ls_number_reflns         11584
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0255
_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^)+(0.0185P)^2^+3.9939P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0493
_refine_ls_wR_factor_ref         0.0550
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9051
_reflns_number_total             11584
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00344_si_002.cif
_cod_data_source_block           mf896_0m
_cod_database_code               4087587
_shelx_estimated_absorpt_t_max   0.808
_shelx_estimated_absorpt_t_min   0.691
_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.a Secondary CH2 refined with riding coordinates:
 C39(H39A,H39B), C97(H97A,H97B), C98(H98A,H98B)
2.b Aromatic/amide H refined with riding coordinates:
 C34(H34), C16(H16), C45(H45), C11(H11), C10(H10), C06(H06), C33(H33),
 C02(H02), C08(H08), C36(H36), C04(H04), C05(H05), C18(H18), C27(H27), C25(H25),
  C03(H03), C42(H42), C43(H43), C41(H41), C44(H44)
2.c Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C), C13(H13A,H13B,H13C), C90(H90A,H90B,H90C), C99(H99A,H99B,
 H99C), C29(H29A,H29B,H29C), C93(H93A,H93B,H93C), C30(H30A,H30B,H30C), C20(H20A,
 H20B,H20C), C21(H21A,H21B,H21C), C96(H96A,H96B,H96C), C31(H31A,H31B,H31C),
 C92(H92A,H92B,H92C), C22(H22A,H22B,H22C), C95(H95A,H95B,H95C), C91(H91A,H91B,
 H91C), C94(H94A,H94B,H94C)
;
_shelx_res_checksum              46025
_shelx_hkl_checksum              80436
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'