Dimers of Heptapnictide Anions: As144-and P144-in the Crystal Structures of [Rb(18-crown-6)]4As14·6NH3and [Li(NH3)4]4P14·NH3
Hanauer, Tobias; Aschenbrenner, Jürgen C.; Korber, Nikolaus; Inorganic Chemistry 45 (2006) 6723–6727; doi:10.1021/ic060418j

data_4332473
_publ_section_title
;
 Dimers of Heptapnictide Anions:&#x00A0; As144-and P144-in the Crystal
 Structures of [Rb(18-crown-6)]4As14&#x00B7;6NH3and
 [Li(NH3)4]4P14&#x00B7;NH3
;
_journal_issue                   17
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6723
_journal_page_last               6727
_journal_paper_doi               10.1021/ic060418j
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         'C48 H102 As14 N2 O24 Rb4, 4(H3 N)'
_chemical_formula_sum            'C48 H114 As14 N6 O24 Rb4'
_chemical_formula_weight         2550.21
_chemical_name_systematic
; 
 Tetrakis[(1,4,7,10,13,16-Hexaoxacyclooctadecan)Rubidium]
 Tetradekaarsenide-Ammonia(1/6) 
;
_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                 100.640(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.4150(10)
_cell_length_b                   17.2910(10)
_cell_length_c                   25.573(2)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      25.96
_cell_measurement_theta_min      2.00
_cell_volume                     4526.2(6)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0643
_diffrn_reflns_av_sigmaI/netI    0.0622
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            41318
_diffrn_reflns_theta_full        25.96
_diffrn_reflns_theta_max         25.96
_diffrn_reflns_theta_min         2.00
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.291
_exptl_absorpt_correction_T_max  0.558
_exptl_absorpt_correction_T_min  0.249
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'DelREFABS in Platon for Windows'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.871
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       collum
_exptl_crystal_F_000             2492
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.452
_refine_diff_density_min         -0.413
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.806
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     493
_refine_ls_number_reflns         8803
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.806
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0284
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0241P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0529
_refine_ls_wR_factor_ref         0.0564
_reflns_number_gt                5827
_reflns_number_total             8803
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060418jsup1.cif
_cod_data_source_block           C48H114As14N6O24Rb4
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4332473