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_4342384
_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         'C25 H46 P2 Rh Ta'
_chemical_formula_sum            'C25 H46 P2 Rh Ta'
_chemical_formula_weight         692.42
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 96.1801(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1777(8)
_cell_length_b                   11.7214(9)
_cell_length_c                   20.3760(15)
_cell_measurement_reflns_used    9995
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      30.21
_cell_measurement_theta_min      2.53
_cell_volume                     2654.1(3)
_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      90.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_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  0.0297
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            30711
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         30.219
_diffrn_reflns_theta_min         1.832
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.872
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.5690
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0758 before and 0.0388 after correction.
The Ratio of minimum to maximum transmission is 0.7627.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.733
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.369
_refine_diff_density_min         -0.669
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     294
_refine_ls_number_reflns         7829
_refine_ls_number_restraints     387
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0280
_refine_ls_R_factor_gt           0.0212
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0132P)^2^+2.3266P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0403
_refine_ls_wR_factor_ref         0.0425
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6897
_reflns_number_total             7829
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic502976r_si_002.cif
_cod_data_source_block           mf1018
_cod_depositor_comments
'Adding full bibliography for 4342380--4342385.cif.'
_cod_database_code               4342384
_shelxl_version_number           2014/6
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H10(0.02) H06(0.021) H19A(0.039) H19B(0.039) H19C(0.039)
 H17A(0.043) H17B(0.043) H17C(0.043) H23A(0.049) H23B(0.049) H23C(0.049)
 H11A(0.021) H11B(0.021) H07(0.023) H03(0.027) H12A(0.028) H12B(0.028)
 H05(0.025) H09(0.021) H04(0.027) H13A(0.027) H13B(0.027) H08(0.023)
 H25A(0.043) H25B(0.043) H25C(0.043) H01(0.024) H02(0.026) H18(0.022)
 H24(0.028) H21(0.024) H15(0.024) H16A(0.036) H16B(0.036) H16C(0.036)
 H14A(0.04) H14B(0.04) H14C(0.04) H20A(0.042) H20B(0.042) H20C(0.042)
 H22A(0.048) H22B(0.048) H22C(0.048) H12C(0.022) H12D(0.022) H13C(0.027)
 H13D(0.027) H11C(0.021) H11D(0.021)
 Fixed X: H10(0.8834) H06(0.7429) H19A(0.7806) H19B(0.745) H19C(0.8306)
 H17A(1.0354) H17B(1.0904) H17C(0.9893) H23A(0.5212) H23B(0.5119) H23C(0.393)
 H11A(0.9057) H11B(0.7925) H07(0.5406) H03(0.6699) H12A(0.7431) H12B(0.7803)
 H05(1.0011) H09(0.7584) H04(0.8547) H13A(0.5901) H13B(0.5664) H08(0.5484)
 H25A(0.3234) H25B(0.3705) H25C(0.4511) H01(0.9068) H02(0.7077) H18(0.9528)
 H24(0.401) H21(0.5266) H15(1.0683) H16A(0.9529) H16B(0.9625) H16C(1.0811)
 H14A(1.1676) H14B(1.1111) H14C(1.0452) H20A(0.7121) H20B(0.7346) H20C(0.6545)
 H22A(0.4482) H22B(0.3979) H22C(0.5038) H12C(0.7035) H12D(0.6848) H13C(0.5582)
 H13D(0.6757) H11C(0.8766) H11D(0.894)
 Fixed Y: H10(0.1597) H06(0.3166) H19A(0.6143) H19B(0.4917) H19C(0.5745)
 H17A(0.6242) H17B(0.5504) H17C(0.6443) H23A(0.4128) H23B(0.5169) H23C(0.4682)
 H11A(0.5626) H11B(0.5927) H07(0.231) H03(-0.1393) H12A(0.5627) H12B(0.4317)
 H05(0.0172) H09(-0.0234) H04(-0.1226) H13A(0.5335) H13B(0.4674) H08(0.02)
 H25A(0.2752) H25B(0.2081) H25C(0.2121) H01(0.0771) H02(-0.0208) H18(0.4395)
 H24(0.3996) H21(0.1641) H15(0.4405) H16A(0.2393) H16B(0.3578) H16C(0.2842)
 H14A(0.2726) H14B(0.3419) H14C(0.2299) H20A(0.245) H20B(0.1598) H20C(0.1199)
 H22A(0.2093) H22B(0.2986) H22C(0.3351) H12C(0.6326) H12D(0.5715) H13C(0.505)
 H13D(0.4452) H11C(0.5076) H11D(0.6012)
 Fixed Z: H10(-0.0679) H06(-0.0353) H19A(0.0683) H19B(0.0377) H19C(0.0013)
 H17A(0.0591) H17B(0.1212) H17C(0.1299) H23A(0.0494) H23B(0.0993) H23C(0.058)
 H11A(0.2343) H11B(0.1827) H07(-0.0245) H03(0.0701) H12A(0.2931) H12B(0.2869)
 H05(0.0694) H09(-0.0805) H04(0.0072) H13A(0.2017) H13B(0.2676) H08(-0.048)
 H25A(0.0785) H25B(0.1446) H25C(0.0843) H01(0.173) H02(0.1729) H18(0.0546)
 H24(0.1666) H21(0.2218) H15(0.2112) H16A(0.2531) H16B(0.2923) H16C(0.2854)
 H14A(0.1809) H14B(0.1173) H14C(0.1404) H20A(0.317) H20B(0.2582) H20C(0.3146)
 H22A(0.32) H22B(0.2644) H22C(0.3196) H12C(0.234) H12D(0.1636) H13C(0.2463)
 H13D(0.2823) H11C(0.2613) H11D(0.2056)
;
_shelx_res_checksum              30309
_shelx_hkl_checksum              35027
_olex2_submission_special_instructions 'No special instructions were received'