Anionic Tantalum Dihydride Complexes: Heterobimetallic Coupling Reactions and Reactivity toward Small-Molecule Activation.
Ostapowicz, Thomas G.; Fryzuk, Michael D.; Inorganic chemistry 54 (2015) 2357–; doi:10.1021/ic502976r

data_4342383
_publ_section_title
;
 Anionic Tantalum Dihydride Complexes: Heterobimetallic Coupling Reactions
 and Reactivity toward Small-Molecule Activation.
;
_journal_issue                   5
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2357
_journal_paper_doi               10.1021/ic502976r
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C10 H12 Ta, C18 H36 N2 Na O6'
_chemical_formula_sum            'C28 H48 N2 Na O6 Ta'
_chemical_formula_weight         712.62
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2014-11-27
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.25 svn.r3098 for OlexSys, GUI svn.r4951)
;
_cell_angle_alpha                71.661(9)
_cell_angle_beta                 83.878(9)
_cell_angle_gamma                60.513(9)
_cell_formula_units_Z            2
_cell_length_a                   11.821(5)
_cell_length_b                   11.840(5)
_cell_length_c                   12.775(5)
_cell_measurement_reflns_used    9436
_cell_measurement_temperature    90
_cell_measurement_theta_max      27.63
_cell_measurement_theta_min      2.24
_cell_volume                     1474.8(11)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      90
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            25707
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.642
_diffrn_reflns_theta_min         1.682
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.784
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5746
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/2 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0840 before and 0.0526 after correction.
The Ratio of minimum to maximum transmission is 0.7707.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_description       plate
_exptl_crystal_F_000             724
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.743
_refine_diff_density_min         -0.728
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     351
_refine_ls_number_reflns         6825
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0191
_refine_ls_R_factor_gt           0.0177
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0146P)^2^+0.4672P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0421
_refine_ls_wR_factor_ref         0.0427
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6502
_reflns_number_total             6825
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic502976r_si_002.cif
_cod_data_source_block           mf1053
_cod_depositor_comments
'Adding full bibliography for 4342380--4342385.cif.'
_cod_original_cell_volume        1474.9(11)
_cod_database_code               4342383
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.566
_shelx_estimated_absorpt_t_min   0.477
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H18A(0.016) H18B(0.016) H28A(0.017) H28B(0.017) H24A(0.016)
 H24B(0.016) H17A(0.016) H17B(0.016) H20A(0.018) H20B(0.018) H12A(0.017)
 H12B(0.017) H11A(0.016) H11B(0.016) H27A(0.018) H27B(0.018) H14A(0.019)
 H14B(0.019) H21A(0.016) H21B(0.016) H23A(0.015) H23B(0.015) H25A(0.017)
 H25B(0.017) H04(0.023) H26A(0.017) H26B(0.017) H13A(0.019) H13B(0.019)
 H19A(0.017) H19B(0.017) H01(0.021) H15A(0.02) H15B(0.02) H22A(0.016)
 H22B(0.016) H16A(0.019) H16B(0.019) H09(0.018) H03(0.021) H07(0.02) H05(0.025)
 H08(0.018) H06(0.021) H02(0.018) H10(0.02)
 Fixed X: H18A(0.4142) H18B(0.3079) H28A(0.824) H28B(0.7899) H24A(0.8727)
 H24B(0.8317) H17A(0.468) H17B(0.4811) H20A(0.3161) H20B(0.3888) H12A(0.5996)
 H12B(0.7464) H11A(0.7984) H11B(0.6777) H27A(0.992) H27B(0.9243) H14A(0.7495)
 H14B(0.8132) H21A(0.4612) H21B(0.6109) H23A(0.6119) H23B(0.6847) H25A(0.9436)
 H25B(0.9871) H04(1.12) H26A(0.9923) H26B(0.838) H13A(0.8102) H13B(0.654)
 H19A(0.2436) H19B(0.3179) H01(0.9952) H15A(0.5925) H15B(0.4961) H22A(0.5863)
 H22B(0.4911) H16A(0.6449) H16B(0.7649) H09(0.9613) H03(1.023) H07(0.5973)
 H05(1.095) H08(0.7931) H06(0.6442) H02(0.9519) H10(0.8715)
 Fixed Y: H18A(0.6159) H18B(0.765) H28A(0.6871) H28B(0.5765) H24A(0.4166)
 H24B(0.3067) H17A(0.7982) H17B(0.6579) H20A(0.8158) H20B(0.886) H12A(0.8791)
 H12B(0.8294) H11A(0.5997) H11B(0.6735) H27A(0.5412) H27B(0.6929) H14A(0.9978)
 H14B(0.8348) H21A(0.6675) H21B(0.5724) H23A(0.4649) H23B(0.4529) H25A(0.2786)
 H25B(0.3846) H04(0.0843) H26A(0.3728) H26B(0.4284) H13A(0.9202) H13B(1)
 H19A(0.8632) H19B(0.7016) H01(0.1679) H15A(1.0764) H15B(1.0151) H22A(0.7533)
 H22B(0.8617) H16A(0.941) H16B(0.8827) H09(0.2312) H03(-0.0683) H07(0.3285)
 H05(0.2377) H08(0.149) H06(0.5126) H02(-0.0157) H10(0.4538)
 Fixed Z: H18A(0.6146) H18B(0.6202) H28A(0.0675) H28B(0.1511) H24A(0.6781)
 H24B(0.6763) H17A(0.6758) H17B(0.7575) H20A(0.25) H20B(0.2816) H12A(0.6303)
 H12B(0.6681) H11A(0.7096) H11B(0.7785) H27A(0.2062) H27B(0.2138) H14A(0.2933)
 H14B(0.3329) H21A(0.1669) H21B(0.2105) H23A(0.6702) H23B(0.775) H25A(0.5136)
 H25B(0.5212) H04(0.063) H26A(0.3374) H26B(0.3364) H13A(0.4818) H13B(0.4694)
 H19A(0.4188) H19B(0.4393) H01(0.3561) H15A(0.168) H15B(0.1797) H22A(0.0499)
 H22B(0.1118) H16A(0.0489) H16B(0.1339) H09(-0.0784) H03(0.1683) H07(0.0351)
 H05(0.1775) H08(-0.0314) H06(0.0349) H02(0.3495) H10(-0.0308)
;
_shelx_res_checksum              71425
_shelx_hkl_checksum              80419
_olex2_submission_special_instructions 'No special instructions were received'