Unprecedented gallium-nitrogen anions: synthesis and characterization of [(Cl3Ga)3N]^3-^ and [(Cl3Ga)2NSnMe3]^2-^
Robert J. Wilson; Jason R. Jones; Miriam V. Bennett; Chem.Commun. 49 (2013) 5049–; doi:10.1039/c3cc41897a

data_7109333
_publ_section_title
;
 Unprecedented gallium-nitrogen anions: synthesis and characterization of
 [(Cl3Ga)3N]^3-^ and [(Cl3Ga)2NSnMe3]^2-^
;
_journal_name_full               Chem.Commun.
_journal_page_first              5049
_journal_paper_doi               10.1039/c3cc41897a
_journal_volume                  49
_journal_year                    2013
_chemical_formula_moiety         '3(C4 H12 N), Cl9 Ga3 N'
_chemical_formula_sum            'C12 H36 Cl9 Ga3 N4'
_chemical_formula_weight         764.66
_chemical_properties_physical    'air-sensitive, moisture-sensitive'
_space_group_IT_number           146
_symmetry_cell_setting           rhombohedral
_symmetry_Int_Tables_number      146
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   10.7081(18)
_cell_length_b                   10.7081(18)
_cell_length_c                   22.379(4)
_cell_measurement_reflns_used    3500
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.82
_cell_measurement_theta_min      2.38
_cell_volume                     2222.3(7)
_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      100(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0376
_diffrn_reflns_av_sigmaI/netI    0.0374
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            12536
_diffrn_reflns_theta_full        30.48
_diffrn_reflns_theta_max         30.48
_diffrn_reflns_theta_min         2.38
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.529
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6590
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, Acta Cryst. (1995) A51 33'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.714
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'triangular plate'
_exptl_crystal_F_000             1146
_exptl_crystal_recrystallization_method acetontrile/THF
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.331
_refine_diff_density_min         -0.235
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.004(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     141
_refine_ls_number_reflns         2856
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0334
_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^)+(0.0313P)^2^+1.0855P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0644
_refine_ls_wR_factor_ref         0.0689
_reflns_number_gt                2327
_reflns_number_total             2856
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc41897a.txt
_cod_data_source_block           rw45b_0m
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               7109333