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_7124335
_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 H88 B3 N12 Ta3'
_chemical_formula_sum            'C72 H88 B3 N12 Ta3'
_chemical_formula_weight         1696.82
_chemical_name_systematic
'[Bis{bis(3-(2,4,6-trimethylphenyl)-imidazole-2-ylidene)dihydrido)boron-tantalum(III)}-bis(\m-hydrido)]-[([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)-(\m-hydrido)'
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_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_date             2019-07-26
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-08-31 deposited with the CCDC.    2019-10-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.533(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.5383(9)
_cell_length_b                   12.5927(5)
_cell_length_c                   33.4495(14)
_cell_measurement_reflns_used    4810
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.28
_cell_measurement_theta_min      2.41
_cell_volume                     8293.5(6)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.01
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1250
_diffrn_reflns_av_unetI/netI     0.1088
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            80563
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.441
_diffrn_reflns_theta_min         1.270
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.991
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6059
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0892 before and 0.0650 after correction.
The Ratio of minimum to maximum transmission is 0.8131.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_description       needle
_exptl_crystal_F_000             3352
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene, hexane'
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.872
_refine_diff_density_min         -1.206
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     865
_refine_ls_number_reflns         15306
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0935
_refine_ls_R_factor_gt           0.0566
_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^)+31.4752P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0912
_refine_ls_wR_factor_ref         0.1011
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10307
_reflns_number_total             15306
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc07686g7.cif
_cod_data_source_block           jif009
_cod_database_code               7124335
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 B2-H2B
 1 with sigma of 0.02
 Ta2-HD
 1.9 with sigma of 0.02
 Ta1-HD
 1.7 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C65) = Uanis(C67)
Uanis(C65) = Uanis(C67A)
Uanis(C68A) = Uanis(C69A)
Uanis(C70A) = Uanis(C69)
Uanis(C70A) = Uanis(C71)
Uanis(B3) = Uanis(B2)
Uanis(C68) = Uanis(C67)
4. Others
 Sof(C67A)=Sof(H67A)=Sof(C68A)=Sof(C69A)=Sof(H69D)=Sof(H69E)=Sof(H69F)=
 Sof(C70A)=Sof(H70A)=1-FVAR(1)
 Sof(C67)=Sof(H67)=Sof(C68)=Sof(C69)=Sof(H69A)=Sof(H69B)=Sof(H69C)=Sof(C70)=
 Sof(H70)=FVAR(1)
 Fixed Uiso: H(0.007) HA(0.007) HD(0.007)
5.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B)
5.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C11(H11), C14(H14), C19(H19), C22(H22),
 C27(H27), C28(H28), C29(H29), C30(H30), C34(H34), C37(H37), C43(H43), C46(H46),
  C51(H51), C52(H52), C53(H53), C54(H54), C58(H58), C61(H61), C67(H67),
 C67A(H67A), C70(H70), C70A(H70A)
5.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C13(H13A,H13B,H13C), C18(H18A,H18B,H18C), C21(H21A,H21B,
 H21C), C24(H24A,H24B,H24C), C33(H33A,H33B,H33C), C36(H36A,H36B,H36C), C39(H39A,
 H39B,H39C), C42(H42A,H42B,H42C), C45(H45A,H45B,H45C), C48(H48A,H48B,H48C),
 C57(H57A,H57B,H57C), C60(H60A,H60B,H60C), C63(H63A,H63B,H63C), C66(H66A,H66B,
 H66C), C69(H69A,H69B,H69C), C69A(H69D,H69E,H69F), C72(H72A,H72B,H72C)
;
_olex2_submission_special_instructions 'No special instructions were received'