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_4342381
_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         'C22 H36 K O6 Ta'
_chemical_formula_sum            'C22 H36 K O6 Ta'
_chemical_formula_weight         616.56
_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                 99.866(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.139(5)
_cell_length_b                   9.791(5)
_cell_length_c                   22.628(9)
_cell_measurement_reflns_used    9103
_cell_measurement_temperature    90
_cell_measurement_theta_max      30.03
_cell_measurement_theta_min      2.77
_cell_volume                     2431.4(19)
_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 0.996
_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  0.0466
_diffrn_reflns_av_unetI/netI     0.0420
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            27386
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         30.050
_diffrn_reflns_theta_min         1.923
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.725
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.5509
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0748 before and 0.0521 after correction.
The Ratio of minimum to maximum transmission is 0.7385.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.684
_exptl_crystal_description       plate
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.667
_refine_diff_density_min         -1.543
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     279
_refine_ls_number_reflns         7084
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0267
_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^)+(0.0236P)^2^+0.9113P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0554
_refine_ls_wR_factor_ref         0.0581
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6021
_reflns_number_total             7084
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic502976r_si_002.cif
_cod_data_source_block           mf1017
_cod_depositor_comments
'Adding full bibliography for 4342380--4342385.cif.'
_cod_original_cell_volume        2431.3(19)
_cod_database_code               4342381
_shelxl_version_number           2014/6
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H22A(0.027) H22B(0.027) H14A(0.026) H14B(0.026) H20A(0.023)
 H20B(0.023) H07(0.02) H01(0.021) H18A(0.021) H18B(0.021) H17A(0.022)
 H17B(0.022) H04(0.018) H21A(0.024) H21B(0.024) H12A(0.034) H12B(0.034)
 H13A(0.03) H13B(0.03) H11A(0.033) H11B(0.033) H03(0.018) H06(0.021)
 H19A(0.023) H19B(0.023) H10(0.021) H02(0.021) H05(0.019) H08(0.021) H09(0.021)
 H16A(0.024) H16B(0.024) H15A(0.025) H15B(0.025)
 Fixed X: H22A(-0.2646) H22B(-0.3245) H14A(-0.0092) H14B(-0.1257) H20A(0.0064)
 H20B(-0.1131) H07(0.2915) H01(0.057) H18A(0.0978) H18B(-0.0181) H17A(0.166)
 H17B(0.2142) H04(0.4301) H21A(-0.2) H21B(-0.0845) H12A(-0.1174) H12B(-0.2396)
 H13A(-0.1318) H13B(-0.009) H11A(-0.3344) H11B(-0.2945) H03(0.3392) H06(0.2452)
 H19A(-0.1308) H19B(-0.0144) H10(0.3767) H02(0.1084) H05(0.2537) H08(0.4579)
 H09(0.5162) H16A(0.2171) H16B(0.177) H15A(-0.0043) H15B(0.1134)
 Fixed Y: H22A(0.1743) H22B(0.2827) H14A(0.0692) H14B(0.1606) H20A(0.5242)
 H20B(0.6077) H07(0.3628) H01(0.1135) H18A(0.766) H18B(0.7108) H17A(0.6681)
 H17B(0.5764) H04(0.0773) H21A(0.3918) H21B(0.3093) H12A(-0.0426) H12B(-0.0782)
 H13A(-0.0582) H13B(-0.0198) H11A(0.1183) H11B(0.011) H03(-0.0724) H06(0.5175)
 H19A(0.682) H19B(0.7433) H10(0.4481) H02(-0.0481) H05(0.2001) H08(0.195)
 H09(0.2554) H16A(0.376) H16B(0.4841) H15A(0.3588) H15B(0.2661)
 Fixed Z: H22A(0.4406) H22B(0.3909) H14A(0.1406) H14B(0.1475) H20A(0.4451)
 H20B(0.4541) H07(0.3238) H01(0.5032) H18A(0.3137) H18B(0.2678) H17A(0.2302)
 H17B(0.2883) H04(0.5279) H21A(0.4734) H21B(0.4583) H12A(0.3211) H12B(0.275)
 H13A(0.1939) H13B(0.239) H11A(0.3089) H11B(0.3623) H03(0.4381) H06(0.4052)
 H19A(0.3507) H19B(0.3944) H10(0.5032) H02(0.4252) H05(0.565) H08(0.3684)
 H09(0.4804) H16A(0.2206) H16B(0.1675) H15A(0.1361) H15B(0.1334)
;
_shelx_res_checksum              53322
_shelx_hkl_checksum              42402
_olex2_submission_special_instructions 'No special instructions were received'