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_4087585
_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         'C41 H48 N2 P Ta'
_chemical_formula_sum            'C41 H48 N2 P Ta'
_chemical_formula_weight         780.77
_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'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     direct
_audit_creation_date             2015-04-19
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 99.4195(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.4666(5)
_cell_length_b                   12.4000(5)
_cell_length_c                   25.0796(11)
_cell_measurement_reflns_used    9897
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.10
_cell_measurement_theta_min      2.44
_cell_volume                     3517.9(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.9928
_diffrn_measured_fraction_theta_max 0.9928
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0208
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            21985
_diffrn_reflns_theta_full        25.1027
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         1.84
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.201
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6026
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0547 before and 0.0307 after correction.
The Ratio of minimum to maximum transmission is 0.8086.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.4740
_exptl_crystal_description       prism
_exptl_crystal_F_000             1582.5586
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.8355
_refine_diff_density_min         -0.5413
_refine_diff_density_rms         0.0873
_refine_ls_d_res_high            0.8376
_refine_ls_d_res_low             11.0857
_refine_ls_goodness_of_fit_ref   1.0887
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    74
_refine_ls_number_parameters     415
_refine_ls_number_reflns         6227
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0887
_refine_ls_R_factor_all          0.0218
_refine_ls_R_factor_gt           0.0185
_refine_ls_shift/su_max          0.0098
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0113P)^2^+4.3562P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0394
_refine_ls_wR_factor_ref         0.0406
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              11
_reflns_limit_h_min              -13
_reflns_limit_k_max              14
_reflns_limit_k_min              0
_reflns_limit_l_max              29
_reflns_limit_l_min              -10
_reflns_number_gt                5726
_reflns_number_total             6227
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            om5b00344_si_002.cif
_cod_data_source_block           mf890_0m
_cod_original_cell_volume        3518(2)
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_database_code               4087585
_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 Me refined with riding coordinates:
 C41(H41a,H41b,H41c)
2.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C33(H33), C25(H25), C02(H02), C34(H34), C36(H36), C16(H16),
 C10(H10), C06(H06), C04(H04), C08(H08), C05(H05), C27(H27), C18(H18), C03(H03)
2.c Idealised Me refined as rotating group:
 C40(H40a,H40b,H40c), C31(H31a,H31b,H31c), C13(H13a,H13b,H13c), C30(H30a,H30b,
 H30c), C38(H38a,H38b,H38c), C29(H29a,H29b,H29c), C20(H20a,H20b,H20c), C39(H39a,
 H39b,H39c), C22(H22a,H22b,H22c), C21(H21a,H21b,H21c)
;
_olex2_submission_special_instructions 'No special instructions were received'