A Tripodal Ligand Constructed from Mesoionic Carbene Donors
Wei-Tsung Lee; Diane A. Dickie; Alejandro J. Metta-Magaña; Jeremy M. Smith; Inorganic Chemistry 52 (2013) 12842–12846; doi:10.1021/ic402311c

data_4336675
_publ_section_title
;
 A Tripodal Ligand Constructed from Mesoionic Carbene Donors
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12842
_journal_page_last               12846
_journal_paper_doi               10.1021/ic402311c
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C60 H59 B N10 Ni O'
_chemical_formula_weight         1005.69
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 115.455(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   31.314(5)
_cell_length_b                   15.180(3)
_cell_length_c                   31.542(5)
_cell_measurement_reflns_used    5296
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      20.60
_cell_measurement_theta_min      2.78
_cell_volume                     13538(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0835
_diffrn_reflns_av_sigmaI/netI    0.0874
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            63865
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         1.44
_exptl_absorpt_coefficient_mu    0.327
_exptl_absorpt_correction_T_max  0.9508
_exptl_absorpt_correction_T_min  0.8687
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker, SADABS'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    0.987
_exptl_crystal_description       irregular
_exptl_crystal_F_000             4240
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.646
_refine_diff_density_min         -0.529
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.968
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     651
_refine_ls_number_reflns         12860
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.968
_refine_ls_R_factor_all          0.1116
_refine_ls_R_factor_gt           0.0668
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1220P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1914
_refine_ls_wR_factor_ref         0.2080
_reflns_number_gt                7330
_reflns_number_total             12860
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic402311c_si_001_1.cif
_cod_data_source_block           jsnmsuwtl21_0m_sqr
_cod_database_code               4336675