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_7124337
_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 H68 B2 Cl2 N8 Ta2, C7 H8'
_chemical_formula_sum            'C55 H68 B2 Cl2 N8 Ta2'
_chemical_formula_weight         1295.59
_chemical_name_systematic
Bis[(bis(3-(2,4,6-trimethylphenyl)-imidazole-2-ylidene)dihydrido)boron-chlorido-tantalum(IV)]-tetrakis(\m-hydrido)
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_chemical_temperature_decomposition 439
_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                 96.747(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.6448(3)
_cell_length_b                   17.7225(4)
_cell_length_c                   18.6699(4)
_cell_measurement_reflns_used    27791
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.6950
_cell_measurement_theta_min      3.2950
_cell_volume                     5469.2(2)
_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  0.0653
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            72862
_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         3.180
_diffrn_source                   'Rotating-anode X-Ray tube'
_exptl_absorpt_coefficient_mu    4.140
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68207
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.37b (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_description       block
_exptl_crystal_F_000             2576
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene, hexane'
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.060
_refine_diff_density_max         2.074
_refine_diff_density_min         -1.248
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         11163
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0268
_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^)+(0.0212P)^2^+6.5258P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0621
_refine_ls_wR_factor_ref         0.0654
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9142
_reflns_number_total             11163
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc07686g7.cif
_cod_data_source_block           jif006
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' tag was changed to
'_chemical_temperature_decomposition' since the value had been '439
(decomp)'. The value '439 (decomp)' was changed to '439'.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_database_code               7124337
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.491
_shelx_estimated_absorpt_t_max   0.789
_shelx_res_checksum              99955