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_4310728
_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            'As3 Ca H43 N14 S6'
_chemical_formula_weight         696.68
_chemical_name_systematic
;
  Ammonium Dicalcium Hexathiotriarsenate(III)-Ammonia(1/13)
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.1920(10)
_cell_length_b                   12.4280(10)
_cell_length_c                   19.3960(10)
_cell_measurement_temperature    123(2)
_cell_volume                     2938.9(4)
_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 0.936
_diffrn_measured_fraction_theta_max 0.936
_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  0.0601
_diffrn_reflns_av_sigmaI/netI    0.0892
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11988
_diffrn_reflns_theta_full        25.93
_diffrn_reflns_theta_max         25.93
_diffrn_reflns_theta_min         2.10
_exptl_absorpt_coefficient_mu    4.007
_exptl_absorpt_correction_type   refdelf
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.575
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1424
_refine_diff_density_max         0.329
_refine_diff_density_min         -0.358
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.010(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.773
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         5137
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      0.773
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0332
_refine_ls_shift/su_max          1.731
_refine_ls_shift/su_mean         0.097
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0184P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0511
_refine_ls_wR_factor_ref         0.0544
_reflns_number_gt                3940
_reflns_number_total             5137
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035175zsi20031017_121809_2.cif
_cod_data_source_block           a
_cod_original_formula_sum        'H43 As3 Ca N14 S6'
_cod_database_code               4310728