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_7124341
_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         'C27 H37 B Cl N4 Ta'
_chemical_formula_sum            'C27 H37 B Cl N4 Ta'
_chemical_formula_weight         644.81
_chemical_name_systematic
(Bis(3-(2,4,6-trimethylphenyl)-imidazole-2-ylidene)dihydrido)boron-chloridio-trimethyl-tantalum(V)
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_chemical_temperature_decomposition 416
_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   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-06-14
_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                93.644(2)
_cell_angle_beta                 98.974(2)
_cell_angle_gamma                94.335(2)
_cell_formula_units_Z            2
_cell_length_a                   10.4157(3)
_cell_length_b                   11.4099(3)
_cell_length_c                   12.0668(2)
_cell_measurement_reflns_used    22868
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.6920
_cell_measurement_theta_min      3.6070
_cell_volume                     1408.30(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.37b (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.37b (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.37b (Rigaku OD, 2017)'
_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(2)
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.855
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     24.00  75.00   0.50    0.50    --    2.33  57.00 -30.00  102
  2  \w    -12.00  74.00   0.50    0.50    --    2.33  57.00-150.00  172
  3  \w     22.00  47.00   0.50    0.50    --    2.33  18.00  48.00   50
  4  \w    -71.00  25.00   0.50    0.50    --    2.33 -77.00  90.00  192
  5  \w    -71.00  17.00   0.50    0.50    --    2.33 -57.00   0.00  176
  6  \w    -78.00  14.00   0.50    0.50    --    2.33 -18.00-120.00  184
  7  \w     -9.00  31.00   0.50    0.50    --    2.33 -99.00   0.00   80
  8  \w    -15.00  31.00   0.50    0.50    --   -2.02 -99.00  60.00   92
  9  \w    -15.00  31.00   0.50    0.50    --   -2.02 -99.00 150.00   92
 10  \w    -15.00  31.00   0.50    0.50    --   -2.02 -99.00-150.00   92
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom DW system, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.855
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            31687
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.855
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.692
_diffrn_reflns_theta_min         3.429
_diffrn_source                   'Rotating-anode X-Ray tube'
_exptl_absorpt_coefficient_mu    4.019
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62201
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_description       block
_exptl_crystal_F_000             644
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.639
_refine_diff_density_min         -0.565
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         6830
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0209
_refine_ls_R_factor_gt           0.0191
_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^)+(0.0244P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0455
_refine_ls_wR_factor_ref         0.0460
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6424
_reflns_number_total             6830
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc07686g7.cif
_cod_data_source_block           jif002
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' tag was changed to
'_chemical_temperature_decomposition' since the value had been '416
(decomp)'. The value '416 (decomp)' was changed to '416'.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_database_code               7124341
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H,H) groups, {H26A,H26B,H26C} of C26, {H27A,H27B,H27C} of C27, All
  C(H) groups
 At 1.5 times of:
  {H21A,H21B,H21C} of C21, {H18A,H18B,H18C} of C18, {H1C,H1D,H1E} of C1, {H5A,
  H5B,H5C} of C5, {H25A,H25B,H25C} of C25, {H24A,H24B,H24C} of C24, {H8A,H8B,
  H8C} of C8
2.a Secondary CH2 refined with riding coordinates:
 B1(H1A,H1B)
2.b Aromatic/amide H refined with riding coordinates:
 C22(H22), C13(H13), C14(H14), C11(H11), C10(H10), C19(H19), C9(H9), C3(H3)
2.c Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C26(H26A,H26B,H26C), C25(H25A,H25B,H25C), C24(H24A,H24B,
 H24C), C18(H18A,H18B,H18C), C8(H8A,H8B,H8C), C21(H21A,H21B,H21C), C1(H1C,H1D,
 H1E), C5(H5A,H5B,H5C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;