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_4342380
_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 K N2 O6, C4 H8 O'
_chemical_formula_sum            'C32 H56 K N2 O7 Ta'
_chemical_formula_weight         800.83
_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                 92.0870(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1731(4)
_cell_length_b                   32.8881(14)
_cell_length_c                   10.3502(5)
_cell_measurement_reflns_used    9925
_cell_measurement_temperature    90
_cell_measurement_theta_max      29.89
_cell_measurement_theta_min      2.33
_cell_volume                     3460.6(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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0560
_diffrn_reflns_av_unetI/netI     0.0551
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            39491
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         29.911
_diffrn_reflns_theta_min         1.238
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.343
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.5801
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0779 before and 0.0525 after correction.
The Ratio of minimum to maximum transmission is 0.7776.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.616
_refine_diff_density_min         -1.239
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     396
_refine_ls_number_reflns         10027
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0312
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0121P)^2^+1.1341P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0507
_refine_ls_wR_factor_ref         0.0545
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7909
_reflns_number_total             10027
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic502976r_si_002.cif
_cod_data_source_block           mf1006
_cod_depositor_comments
'Adding full bibliography for 4342380--4342385.cif.'
_cod_database_code               4342380
_shelxl_version_number           2014/6
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H28A(0.018) H28B(0.018) H21A(0.018) H21B(0.018) H17A(0.016)
 H17B(0.016) H12A(0.016) H12B(0.016) H2(0.023) H23A(0.02) H23B(0.02) H31A(0.02)
 H31B(0.02) H10(0.02) H27A(0.019) H27B(0.019) H1(0.025) H32A(0.025) H32B(0.025)
 H7(0.02) H15A(0.019) H15B(0.019) H4(0.02) H6(0.023) H13A(0.02) H13B(0.02)
 H20A(0.017) H20B(0.017) H5(0.024) H19A(0.017) H19B(0.017) H8(0.018) H3(0.023)
 H30A(0.024) H30B(0.024) H9(0.019) H11A(0.018) H11B(0.018) H29A(0.021)
 H29B(0.021) H14A(0.022) H14B(0.022) H25A(0.019) H25B(0.019) H22A(0.017)
 H22B(0.017) H24A(0.02) H24B(0.02) H16A(0.016) H16B(0.016) H26A(0.018)
 H26B(0.018) H18A(0.018) H18B(0.018)
 Fixed X: H28A(0.3301) H28B(0.4337) H21A(0.1783) H21B(0.3092) H17A(-0.0766)
 H17B(-0.0052) H12A(-0.1828) H12B(-0.2413) H2(-0.3407) H23A(0.2064)
 H23B(0.1001) H31A(0.4189) H31B(0.5556) H10(-0.3218) H27A(0.4978) H27B(0.5248)
 H1(-0.4943) H32A(0.5127) H32B(0.6128) H7(-0.24) H15A(0.1188) H15B(0.0081) H4(-
 0.1258) H6(-0.4074) H13A(-0.2463) H13B(-0.1966) H20A(0.2439) H20B(0.1054) H5(-
 0.3664) H19A(0.1674) H19B(0.2878) H8(-0.047) H3(-0.111) H30A(0.5559)
 H30B(0.4378) H9(-0.0938) H11A(-0.0488) H11B(-0.1275) H29A(0.6863) H29B(0.5734)
 H14A(-0.1508) H14B(-0.0578) H25A(0.408) H25B(0.2991) H22A(0.4273) H22B(0.3584)
 H24A(0.1506) H24B(0.2755) H16A(0.1248) H16B(0.2094) H26A(0.5051) H26B(0.5021)
 H18A(0.193) H18B(0.0825)
 Fixed Y: H28A(0.2479) H28B(0.24) H21A(0.1572) H21B(0.1374) H17A(0.041)
 H17B(0.0124) H12A(0.0973) H12B(0.1202) H2(0.0437) H23A(0.0421) H23B(0.0444)
 H31A(0.063) H31B(0.0856) H10(0.2081) H27A(0.1792) H27B(0.218) H1(0.0723)
 H32A(0.0044) H32B(0.0355) H7(0.1868) H15A(0.2546) H15B(0.2593) H4(0.1083)
 H6(0.2141) H13A(0.1829) H13B(0.1638) H20A(0.0726) H20B(0.0863) H5(0.1138)
 H19A(0.0221) H19B(0.043) H8(0.162) H3(0.0666) H30A(0.0686) H30B(0.0381)
 H9(0.1764) H11A(0.1039) H11B(0.0649) H29A(0.0147) H29B(-0.0142) H14A(0.2345)
 H14B(0.2256) H25A(0.1392) H25B(0.1707) H22A(0.1721) H22B(0.2024) H24A(0.113)
 H24B(0.0856) H16A(0.2155) H16B(0.2539) H26A(0.1869) H26B(0.1455) H18A(0.0207)
 H18B(0.0004)
 Fixed Z: H28A(0.6072) H28B(0.5015) H21A(0.2902) H21B(0.244) H17A(0.7006)
 H17B(0.8017) H12A(0.7171) H12B(0.8355) H2(0.1587) H23A(0.8874) H23B(0.9928)
 H31A(0.6936) H31B(0.7089) H10(0.3613) H27A(0.6109) H27B(0.6966) H1(0.3145)
 H32A(0.6296) H32B(0.5719) H7(-0.0137) H15A(0.6072) H15B(0.4982) H4(0.4268)
 H6(0.1307) H13A(0.7363) H13B(0.6077) H20A(0.2821) H20B(0.3286) H5(0.4785)
 H19A(0.4151) H19B(0.4879) H8(0.1209) H3(0.2207) H30A(0.9183) H30B(0.8947)
 H9(0.3556) H11A(0.96) H11B(0.917) H29A(0.9314) H29B(0.8777) H14A(0.6225)
 H14B(0.744) H25A(1.0254) H25B(0.9814) H22A(0.409) H22B(0.3112) H24A(1.0286)
 H24B(1.0543) H16A(0.3639) H16B(0.4003) H26A(0.8967) H26B(0.8212) H18A(0.691)
 H18B(0.6023)
;
_shelx_res_checksum              69384
_shelx_hkl_checksum              86722
_olex2_submission_special_instructions 'No special instructions were received'