Structural diversity in multinuclear tantalum polyhydrides formed via reductive hydrogenolysis of metal‒carbon bonds
Fostvedt, Jade I.; Lohrey, Trevor D.; Bergman, Robert G.; Arnold, John; Chemical Communications  (2019) –; doi:10.1039/C9CC07686G

data_7124338
_publ_section_title
;
 Structural diversity in multinuclear tantalum polyhydrides formed via
 reductive hydrogenolysis of metal--carbon bonds
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC07686G
_journal_year                    2019
_chemical_formula_moiety
'C55 H66 B2 N8 Ta2, C55 H66 B2 N8 Ta2, C55 H66 B2 N8 Ta2, C6 H14, C6 H14, C6 H14'
_chemical_formula_sum            'C183 H240 B6 N24 Ta6'
_chemical_formula_weight         3926.54
_chemical_name_systematic
'Bis[(bis(3-(2,4,6-trimethylphenyl)-imidazole-2-ylidene)dihydrido)boron-tantalum(III)]-bis(\m-hydrido)-( \m-\h4:\h4-toluene)'
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_chemical_temperature_decomposition 447
_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
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-08-31 deposited with the CCDC.    2019-10-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.941(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.8721(4)
_cell_length_b                   28.0792(8)
_cell_length_c                   44.8293(12)
_cell_measurement_reflns_used    9920
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.09
_cell_measurement_theta_min      2.36
_cell_volume                     17459.4(8)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.0742
_diffrn_reflns_av_unetI/netI     0.0476
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       56
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_number            278605
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_min         0.856
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    3.802
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5793
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_description       Prism
_exptl_crystal_F_000             7896
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene, hexane'
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.126
_refine_diff_density_min         -1.236
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2125
_refine_ls_number_reflns         35701
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0369
_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^)+59.0796P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0620
_refine_ls_wR_factor_ref         0.0660
_reflns_Friedel_coverage         0.000
_reflns_number_gt                29241
_reflns_number_total             35701
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc07686g7.cif
_cod_data_source_block           jif011_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' tag was changed to
'_chemical_temperature_decomposition' since the value had been '447
(decomp)'. The value '447 (decomp)' was changed to '447'.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_database_code               7124338
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.517
_shelx_estimated_absorpt_t_min   0.450
_shelx_res_checksum              4124