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_7124340
_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         'C54 H64 B2 N8 Ta2'
_chemical_formula_sum            'C54 H64 B2 N8 Ta2'
_chemical_formula_weight         1208.65
_chemical_name_systematic
'Bis[(bis(3-(2,4,6-trimethylphenyl)-imidazole-2-ylidene)dihydrido)boron-tantalum(III)]-bis(\m-hydrido)-( \m-\h4:\h4-benzene)'
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_chemical_temperature_decomposition 462
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_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                86.292(2)
_cell_angle_beta                 83.751(2)
_cell_angle_gamma                66.080(2)
_cell_formula_units_Z            2
_cell_length_a                   12.8612(3)
_cell_length_b                   12.8924(3)
_cell_length_c                   16.4689(4)
_cell_measurement_reflns_used    35652
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.7890
_cell_measurement_theta_min      3.1490
_cell_volume                     2480.73(11)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'ROD, Synergy Custom DW system, Pilatus 200K'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0605
_diffrn_reflns_av_unetI/netI     0.0434
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            52257
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.112
_diffrn_source                   'Rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    4.453
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48065
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.45f (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.618
_exptl_crystal_description       plate
_exptl_crystal_F_000             1200
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene, hexane'
_exptl_crystal_size_max          0.410
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.050
_refine_diff_density_max         2.165
_refine_diff_density_min         -1.803
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     639
_refine_ls_number_reflns         10138
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0372
_refine_ls_R_factor_gt           0.0319
_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^)+(0.0438P)^2^+0.3368P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0784
_refine_ls_wR_factor_ref         0.0802
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8861
_reflns_number_total             10138
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc07686g7.cif
_cod_data_source_block           jif008
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' tag was changed to
'_chemical_temperature_decomposition' since the value had been '462
(decomp)'. The value '462 (decomp)' was changed to '462'.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        2480.75(12)
_cod_database_code               7124340
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.263
_shelx_estimated_absorpt_t_max   0.808
_shelx_res_checksum              65938