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_4342382
_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         'C38 H50 K4 O2 Ta2'
_chemical_formula_sum            'C38 H50 K4 O2 Ta2'
_chemical_formula_weight         1057.08
_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             2014-11-27
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.25 svn.r3098 for OlexSys, GUI svn.r4951)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.4808(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2395(5)
_cell_length_b                   15.3764(7)
_cell_length_c                   23.2419(9)
_cell_measurement_reflns_used    8943
_cell_measurement_temperature    90
_cell_measurement_theta_max      29.49
_cell_measurement_theta_min      2.24
_cell_volume                     4016.6(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
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.983
_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  0.0512
_diffrn_reflns_av_unetI/netI     0.0454
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            44349
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         29.662
_diffrn_reflns_theta_min         1.588
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.889
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.5482
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0807 before and 0.0620 after correction. The Ratio of minimum to maximum transmission is 0.7350. The \l/2 correction factor is 0.0015.'
_exptl_crystal_density_diffrn    1.748
_exptl_crystal_description       Plate
_exptl_crystal_F_000             2064
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.187
_refine_diff_density_min         -1.684
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         11171
_refine_ls_number_restraints     1131
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0276
_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^)+(0.0078P)^2^+6.3792P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0549
_refine_ls_wR_factor_ref         0.0582
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9384
_reflns_number_total             11171
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic502976r_si_002.cif
_cod_data_source_block           mf1019
_cod_depositor_comments
'Adding full bibliography for 4342380--4342385.cif.'
_cod_database_code               4342382
_shelxl_version_number           2014/6
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H01(0.018) H02(0.018) H03(0.018) H04(0.018) H05(0.018) H06(0.022)
 H07(0.024) H08(0.021) H09(0.02) H10(0.02) H11(0.023) H12(0.02) H13(0.02)
 H14(0.021) H15(0.024) H16(0.022) H17(0.019) H18(0.018) H19(0.02) H20(0.02)
 H21(0.026) H22(0.027) H23(0.025) H24(0.023) H25(0.024) H26(0.035) H27(0.042)
 H28(0.044) H29(0.033) H30(0.027) H31A(0.082) H31B(0.082) H32A(0.091)
 H32B(0.091) H33A(0.073) H33B(0.073) H34A(0.059) H34B(0.059) H35A(0.062)
 H35B(0.062) H35C(0.062) H35D(0.062) H36A(0.073) H36B(0.073) H36C(0.073)
 H36D(0.073) H37A(0.097) H37B(0.097) H37C(0.097) H37D(0.097) H38A(0.071)
 H38B(0.071) H38C(0.071) H38D(0.071) H34C(0.059) H34D(0.059) H31C(0.082)
 H31D(0.082) H32C(0.091) H32D(0.091) H33C(0.073) H33D(0.073)
 Fixed X: H01(0.693) H02(0.612) H03(0.5462) H04(0.5891) H05(0.685) H06(1.0504)
 H07(0.9405) H08(0.7546) H09(0.7542) H10(0.9337) H11(0.2072) H12(0.1047)
 H13(0.2418) H14(0.4173) H15(0.395) H16(0.7244) H17(0.8542) H18(1.0466)
 H19(1.0347) H20(0.8413) H21(0.398) H22(0.3757) H23(0.195) H24(0.1045)
 H25(0.2306) H26(0.8687) H27(1.0266) H28(1.2193) H29(1.1813) H30(0.9643)
 H31A(0.3463) H31B(0.4675) H32A(0.2689) H32B(0.3839) H33A(0.3491) H33B(0.4435)
 H34A(0.5998) H34B(0.5248) H35A(1.277) H35B(1.2488) H35C(1.2495) H35D(1.3247)
 H36A(1.475) H36B(1.3853) H36C(1.4295) H36D(1.465) H37A(1.472) H37B(1.4923)
 H37C(1.448) H37D(1.4556) H38A(1.3139) H38B(1.2982) H38C(1.2754) H38D(1.2445)
 H34C(0.5832) H34D(0.5099) H31C(0.4085) H31D(0.5432) H32C(0.3239) H32D(0.4535)
 H33C(0.3928) H33D(0.3122)
 Fixed Y: H01(-0.0768) H02(-0.1357) H03(-0.0087) H04(0.1323) H05(0.0898)
 H06(0.0383) H07(-0.0061) H08(0.0857) H09(0.1946) H10(0.1599) H11(-0.2176) H12(-
 0.095) H13(-0.0569) H14(-0.163) H15(-0.2583) H16(0.2429) H17(0.1124)
 H18(0.1709) H19(0.3367) H20(0.3805) H21(0.2301) H22(0.1827) H23(0.0856)
 H24(0.0741) H25(0.1613) H26(0.4037) H27(0.3186) H28(0.3393) H29(0.4385)
 H30(0.4772) H31A(-0.1586) H31B(-0.177) H32A(-0.076) H32B(-0.1026) H33A(0.0624)
 H33B(0.0444) H34A(0.0065) H34B(0.0703) H35A(0.2061) H35B(0.2864) H35C(0.2663)
 H35D(0.2954) H36A(0.2258) H36B(0.1649) H36C(0.2753) H36D(0.2501) H37A(0.1062)
 H37B(0.1384) H37C(0.0683) H37D(0.1427) H38A(0.0931) H38B(0.0537) H38C(0.083)
 H38D(0.0592) H34C(-0.0206) H34D(0.0546) H31C(-0.2073) H31D(-0.1937) H32C(-
 0.1592) H32D(-0.1518) H33C(-0.0037) H33D(-0.0031)
 Fixed Z: H01(0.7256) H02(0.8175) H03(0.8812) H04(0.8244) H05(0.7284)
 H06(0.8545) H07(0.944) H08(0.9524) H09(0.8678) H10(0.8045) H11(0.731)
 H12(0.7866) H13(0.8724) H14(0.872) H15(0.7828) H16(1.0211) H17(1.0497)
 H18(1.096) H19(1.0918) H20(1.0458) H21(0.7638) H22(0.66) H23(0.6522)
 H24(0.7516) H25(0.8199) H26(0.8614) H27(0.8105) H28(0.8637) H29(0.9483)
 H30(0.947) H31A(0.6329) H31B(0.598) H32A(0.555) H32B(0.5179) H33A(0.5768)
 H33B(0.5267) H34A(0.5951) H34B(0.637) H35A(1.065) H35B(1.0232) H35C(1.044)
 H35D(0.9886) H36A(1.0344) H36B(1.0703) H36C(0.9783) H36D(1.0438) H37A(1.0237)
 H37B(0.9585) H37C(1.0013) H37D(0.9528) H38A(0.9336) H38B(0.9968) H38C(0.9281)
 H38D(0.994) H34C(0.5874) H34D(0.6227) H31C(0.6558) H31D(0.6297) H32C(0.5664)
 H32D(0.5396) H33C(0.5258) H33D(0.5836)
;
_shelx_res_checksum              66309
_shelx_hkl_checksum              1154
_olex2_submission_special_instructions 'No special instructions were received'