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_7124339
_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         'C72 H86 B3 N12 Ta3, C6 H14'
_chemical_formula_sum            'C78 H100 B3 N12 Ta3'
_chemical_formula_weight         1780.97
_chemical_name_systematic
'[{Bis([3,5-dimethyl-2-(3-{[3-(2,4,6-trimethylphenyl)imidazol-2-ylidene-1-yl]boranyl}imidazol-2-ylidene-1-yl)phenyl]methyl)-tantalum(III)}-bis(\m-hydrido)]-[bis(3-(2,4,6-trimethylphenyl)-imidazole-2-ylidene)dihydrido)boron-tantalum(III)]-bis(\m-hydrido)'
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_chemical_temperature_decomposition 486
_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
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-08-31 deposited with the CCDC.    2019-10-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.900(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.0723(17)
_cell_length_b                   25.671(3)
_cell_length_c                   17.2881(18)
_cell_measurement_reflns_used    102483
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.109
_cell_measurement_theta_min      1.864
_cell_volume                     7567.0(14)
_computing_cell_refinement       'SAINT V8.38A Bruker, Madison WI'
_computing_data_collection       'Bruker APEX3 Bruker, Madison WI'
_computing_data_reduction        'SAINT V8.38A Bruker, Madison WI'
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    SHELXT
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 with PHOTON-II CPAD detector'
_diffrn_measurement_method       '\f and \w shutterless scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7288
_diffrn_reflns_av_R_equivalents  0.0713
_diffrn_reflns_av_unetI/netI     0.0425
_diffrn_reflns_Laue_measured_fraction_full 1.000
_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       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            102483
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.930
_diffrn_reflns_theta_max         26.109
_diffrn_reflns_theta_min         1.864
_diffrn_source                   'Advanced Light Source, station 12.2.1'
_exptl_absorpt_coefficient_mu    4.634
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.5849
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_description       plate
_exptl_crystal_F_000             3544
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene, hexane'
_exptl_crystal_size_max          0.090
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.005
_refine_diff_density_max         3.247
_refine_diff_density_min         -1.329
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     899
_refine_ls_number_reflns         13925
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0343
_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^)+(0.0411P)^2^+15.2755P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0834
_refine_ls_wR_factor_ref         0.0891
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11247
_reflns_number_total             13925
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc07686g7.cif
_cod_data_source_block           jif010
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' tag was changed to
'_chemical_temperature_decomposition' since the value had been '486
(decomp)'. The value '486 (decomp)' was changed to '486'.

'_atom_sites_solution_secondary' value 'diffmap' was changed to
'difmap'.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        7567.1(13)
_cod_database_code               7124339
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              41406