Structural distortions in M[E(SiMe₃)₂]₃ complexes (M = group 15, f-element; E = N, CH): is three a crowd?
Boyde, Nicholas C.; Chmely, Stephen C.; Hanusa, Timothy P.; Rheingold, Arnold L.; Brennessel, William W.; Inorganic chemistry 53 (2014) 9703–9714; doi:10.1021/ic501232z

data_4340978
_publ_section_title
;
 Structural distortions in M[E(SiMe&#x2083;)&#x2082;]&#x2083; complexes (M
 = group 15, f-element; E = N, CH): is three a crowd?
;
_journal_issue                   18
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9703
_journal_page_last               9714
_journal_paper_doi               10.1021/ic501232z
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C20 H54 N3 Sb Si6, 0.5(C2 H19 N Si2)'
_chemical_formula_sum            'C21 H63.5 N3.5 Sb Si7'
_chemical_formula_weight         683.63
_chemical_name_common            hannb01
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_Hall           '-P 3'
_space_group_name_H-M_alt        'P -3'
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   16.0906(10)
_cell_length_b                   16.0906(10)
_cell_length_c                   8.4214(5)
_cell_measurement_reflns_used    3989
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      29.46
_cell_measurement_theta_min      2.53
_cell_volume                     1888.2(2)
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_collection       'APEX2 (Bruker, 2013)'
_computing_data_reduction        'SAINT (Bruker, 2013)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SIR2011 (Burla et al., 2012)'
_diffrn_ambient_temperature      100.0(5)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD platform'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0606
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            37899
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        33.730
_diffrn_reflns_theta_max         33.724
_diffrn_reflns_theta_min         2.418
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.968
_exptl_absorpt_correction_T_max  0.7467
_exptl_absorpt_correction_T_min  0.6419
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2012)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.202
_exptl_crystal_description       block
_exptl_crystal_F_000             726
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.987
_refine_diff_density_min         -0.990
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     157
_refine_ls_number_reflns         5043
_refine_ls_number_restraints     77
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0596
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1004P)^2^+1.4255P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1522
_refine_ls_wR_factor_ref         0.1635
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4407
_reflns_number_total             5043
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic501232z_si_002.cif
_cod_data_source_block           hannb01
_cod_depositor_comments
'Adding full bibliography for 4340976--4340978.cif.'
_cod_original_cell_volume        1888.2(3)
_cod_original_formula_sum        'C21 H63.50 N3.50 Sb Si7'
_cod_database_code               4340978
_shelx_estimated_absorpt_t_min   0.801
_shelx_estimated_absorpt_t_max   0.861