Tungsten(VI) metallacarborane imido complexes; hydrogen bonding to a bent imido ligand in {W(NtBu)2[N(H)C(Me)NHtBu](C2B9H11)} †
Batsanov, Andrei S.; Goeta, Andrés E.; Howard, Judith A. K.; Hughes, Andrew K.; Johnson, Andrew L.; Wade, Ken; Journal of the Chemical Society, Dalton Transactions  (2001) 1210–; doi:10.1039/b100572n

data_7010583
_publ_section_title
;
 Tungsten(VI) metallacarborane imido complexes; hydrogen bonding to a
 bent imido ligand in
 {W(NtBu)2[N(H)C(Me)NHtBu](C2B9H11)}&#x200A;&#x2020;
;
_journal_issue                   8
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1210
_journal_paper_doi               10.1039/b100572n
_journal_year                    2001
_chemical_formula_sum            'C16 H43 B9 N4 W'
_chemical_formula_weight         572.68
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.333(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.825(3)
_cell_length_b                   10.920(2)
_cell_length_c                   13.523(3)
_cell_measurement_reflns_used    631
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      20.74
_cell_measurement_theta_min      13.70
_cell_volume                     2620.8(9)
_computing_cell_refinement       'SMART-NT V5.0 (Bruker, 1998)'
_computing_data_collection       'SMART-NT V5.0 (Bruker, 1998)'
_computing_data_reduction        'SAINT-NT V5.0 (Bruker, 1998)'
_computing_molecular_graphics    'SHELXTL-NT V5.1 (Bruker, 1998)'
_computing_publication_material  'SHELXTL-NT V5.1 (Bruker, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.918
_diffrn_measured_fraction_theta_max 0.918
_diffrn_measurement_device_type  'BRUKER SMART-CCD'
_diffrn_measurement_method       /w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0526
_diffrn_reflns_av_sigmaI/netI    0.0605
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21485
_diffrn_reflns_theta_full        30.50
_diffrn_reflns_theta_max         30.50
_diffrn_reflns_theta_min         1.15
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    4.418
_exptl_absorpt_correction_T_max  0.803
_exptl_absorpt_correction_T_min  0.475
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   XPREP
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       'rectangular prism'
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.774
_refine_diff_density_min         -0.851
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     333
_refine_ls_number_reflns         7346
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.0616
_refine_ls_R_factor_gt           0.0311
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0210P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0505
_refine_ls_wR_factor_ref         0.0560
_reflns_number_gt                5273
_reflns_number_total             7346
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b100572n.txt
_cod_data_source_block           5
_cod_original_cell_volume        2620.7(8)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7010583