First Characterization of the Ammine-Ammonium Complex [{NH4(NH3)4}2(μ-NH3)2]2+ in the Crystal Structure of [NH4(NH3)4][B(C6H5)4].NH3 and the [NH4(NH3)4]+ Complex in [NH4(NH3)4][Ca(NH3)7]As3S6.2NH3 and [NH4(NH3)4][Ba(NH3)8]As3S6.NH3
Thomas Rossmeier; Markus Reil; Nikolaus Korber; Inorganic Chemistry 43 (2004) 2206–2212; doi:10.1021/ic035175z

data_4310727
_publ_contact_author
;
                 Nikolaus Korber
                 Institut  f\"ur Anorganische Chemie
                 Universit\"at Regensburg
                 Universit\"atsstr.31
                 93053 Regensburg
                 Deutschland
;
_publ_contact_author_email       nikolaus.korber@chemie.uni-regensburg.de
_publ_contact_author_fax         '+49 941 9431812'
_publ_contact_author_phone       '+49 941 9434448'
_publ_section_title
;
 First Characterization of the Ammine-Ammonium Complex
 [{NH4(NH3)4}2(\m-NH3)2]2+ in the Crystal Structure of
 [NH4(NH3)4][B(C6H5)4].NH3 and the [NH4(NH3)4]+ Complex in
 [NH4(NH3)4][Ca(NH3)7]As3S6.2NH3 and [NH4(NH3)4][Ba(NH3)8]As3S6.NH3
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2206
_journal_page_last               2212
_journal_paper_doi               10.1021/ic035175z
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C24 H39 B N6'
_chemical_formula_weight         422.42
_chemical_name_systematic
;
  Ammoniumtetraphenylborate-Ammonia(1/5)?
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.924(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.4693(9)
_cell_length_b                   9.9918(4)
_cell_length_c                   21.1440(10)
_cell_measurement_temperature    123(2)
_cell_volume                     2609.2(3)
_computing_cell_refinement       'Stoe IPDS Software Vers2.89'
_computing_data_collection       'Stoe IPDS Software Vers2.89'
_computing_data_reduction        'Stoe IPDS Software Vers2.89'
_computing_publication_material  'CIFTAB in SHELXL 97'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Stoe Imaging Plate Diffraction System'
_diffrn_measurement_method       Phi
_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  0.0925
_diffrn_reflns_av_sigmaI/netI    0.1323
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            20126
_diffrn_reflns_theta_full        25.95
_diffrn_reflns_theta_max         25.95
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    0.065
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.075
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.170
_refine_diff_density_min         -0.121
_refine_diff_density_rms         0.036
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.720
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         5010
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.720
_refine_ls_R_factor_all          0.1142
_refine_ls_R_factor_gt           0.0423
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0265P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0734
_refine_ls_wR_factor_ref         0.0860
_reflns_number_gt                2278
_reflns_number_total             5010
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035175zsi20031017_121809_1.cif
_cod_data_source_block           b
_cod_original_cell_volume        2609.2(2)
_cod_database_code               4310727