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_4342385
_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         'C29 H55 O P2 Ru Ta'
_chemical_formula_sum            'C29 H55 O P2 Ru Ta'
_chemical_formula_weight         763.69
_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_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2014-11-24
_audit_creation_method
;
Olex2 1.2
(compiled 2014.06.27 svn.r2953 for OlexSys, GUI svn.r4855)
;
_cell_angle_alpha                90
_cell_angle_beta                 106.813(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.339(2)
_cell_length_b                   31.978(8)
_cell_length_c                   10.782(3)
_cell_measurement_reflns_used    9915
_cell_measurement_temperature    90
_cell_measurement_theta_max      30.11
_cell_measurement_theta_min      2.35
_cell_volume                     3082.3(13)
_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)'
_diffrn_ambient_temperature      90
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0471
_diffrn_reflns_av_unetI/netI     0.0489
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            32471
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         30.120
_diffrn_reflns_theta_min         1.273
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.160
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.5563
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0733 before and 0.0480 after correction.
The Ratio of minimum to maximum transmission is 0.7457.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.646
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_refine_diff_density_max         3.571
_refine_diff_density_min         -4.121
_refine_diff_density_rms         0.192
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         8987
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.139
_refine_ls_R_factor_all          0.0621
_refine_ls_R_factor_gt           0.0480
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0107P)^2^+25.7938P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0881
_refine_ls_wR_factor_ref         0.0920
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7522
_reflns_number_total             8987
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic502976r_si_002.cif
_cod_data_source_block           mf1016
_cod_depositor_comments
'Adding full bibliography for 4342380--4342385.cif.'
_cod_original_cell_volume        3082.6(13)
_cod_database_code               4342385
_shelxl_version_number           2014/6
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H05(0.03) H06(0.029) H24(0.022) H07(0.029) H14A(0.05) H14B(0.05)
 H14C(0.05) H26A(0.042) H26B(0.042) H26C(0.042) H15(0.027) H18(0.023)
 H13A(0.032) H13B(0.032) H13C(0.032) H08(0.029) H11A(0.034) H11B(0.034)
 H11C(0.034) H12(0.018) H04(0.024) H01(0.029) H10(0.029) H03(0.025) H09(0.029)
 H16A(0.045) H16B(0.045) H16C(0.045) H22A(0.052) H22B(0.052) H22C(0.052)
 H02(0.027) H21(0.027) H28A(0.039) H28B(0.039) H28C(0.039) H17A(0.043)
 H17B(0.043) H17C(0.043) H27(0.022) H23A(0.039) H23B(0.039) H23C(0.039)
 H25A(0.032) H25B(0.032) H25C(0.032) H19A(0.045) H19B(0.045) H19C(0.045)
 H20A(0.048) H20B(0.048) H20C(0.048)
 Fixed X: H05(0.3548) H06(0.0602) H24(0.6652) H07(-0.1327) H14A(0.4095)
 H14B(0.3858) H14C(0.4508) H26A(0.2177) H26B(0.2463) H26C(0.1552) H15(0.1554)
 H18(-0.05) H13A(0.1315) H13B(0.1457) H13C(-0.0033) H08(-0.1804) H11A(0.0063)
 H11B(0.1433) H11C(0.1591) H12(0.2833) H04(0.0992) H01(0.4603) H10(0.141)
 H03(0.0376) H09(-0.0189) H16A(0.2788) H16B(0.105) H16C(0.2261) H22A(0.558)
 H22B(0.4561) H22C(0.6257) H02(0.27) H21(0.388) H28A(0.3226) H28B(0.4803)
 H28C(0.3282) H17A(-0.1335) H17B(-0.0685) H17C(-0.2256) H27(0.4637)
 H23A(0.8363) H23B(0.7589) H23C(0.7066) H25A(0.6116) H25B(0.541) H25C(0.7188)
 H19A(-0.2357) H19B(-0.087) H19C(-0.157) H20A(0.6913) H20B(0.5561) H20C(0.5921)
 Fixed Y: H05(0.2523) H06(0.1193) H24(0.1194) H07(0.1486) H14A(0.1527)
 H14B(0.1063) H14C(0.142) H26A(0.0184) H26B(0.0155) H26C(0.0542) H15(0.1392)
 H18(0.16) H13A(0.026) H13B(0.0745) H13C(0.0574) H08(0.2236) H11A(0.0301)
 H11B(0.0403) H11C(0.0044) H12(0.0579) H04(0.2855) H01(0.2337) H10(0.1768)
 H03(0.2798) H09(0.2403) H16A(0.2046) H16B(0.2013) H16C(0.2088) H22A(-0.0179)
 H22B(-0.0094) H22C(0.0065) H02(0.2503) H21(0.0374) H28A(0.112) H28B(0.0934)
 H28C(0.0712) H17A(0.1119) H17B(0.1585) H17C(0.15) H27(0.0376) H23A(0.095)
 H23B(0.0572) H23C(0.0684) H25A(0.1427) H25B(0.1686) H25C(0.1654) H19A(0.1164)
 H19B(0.097) H19C(0.0769) H20A(0.062) H20B(0.0859) H20C(0.0384)
 Fixed Z: H05(0.9825) H06(0.8675) H24(0.7751) H07(0.6743) H14A(0.2505)
 H14B(0.2965) H14C(0.4017) H26A(0.9139) H26B(0.7748) H26C(0.8083) H15(0.2295)
 H18(0.4336) H13A(0.2208) H13B(0.1891) H13C(0.2167) H08(0.7204) H11A(0.429)
 H11B(0.5539) H11C(0.4555) H12(0.4042) H04(0.8809) H01(0.7986) H10(1.0356)
 H03(0.6346) H09(0.9473) H16A(0.4085) H16B(0.3307) H16C(0.2539) H22A(0.6777)
 H22B(0.7716) H22C(0.8114) H02(0.5883) H21(0.6015) H28A(0.9772) H28B(1.0604)
 H28C(1.0642) H17A(0.2034) H17B(0.2119) H17C(0.2392) H27(0.9298) H23A(0.9661)
 H23B(0.8737) H23C(0.9986) H25A(1.0124) H25B(0.882) H25C(0.9414) H19A(0.4418)
 H19B(0.5384) H19C(0.3979) H20A(0.6538) H20B(0.5535) H20C(0.5271)
;
_shelx_res_checksum              5987
_shelx_hkl_checksum              43080
_olex2_submission_special_instructions 'No special instructions were received'