An isolated cyclo-tetraarsendiide: low temperature synthesis and crystal structure of bis-pentaamminesodium tetraarsendiide‒ammonia (1/3) [Na(NH3)5]2As4·3NH3
Korber, Nikolaus; Reil, Markus; Chemical Communications  (2002) 84–; doi:10.1039/b108879c

data_7114544
_publ_section_title
;
 An isolated cyclo-tetraarsendiide: low temperature synthesis and crystal
 structure of bis-pentaamminesodium tetraarsendiide--ammonia (1/3)
 [Na(NH3)5]2As4&#x00B7;3NH3
;
_journal_issue                   1
_journal_name_full               'Chemical Communications'
_journal_page_first              84
_journal_paper_doi               10.1039/b108879c
_journal_year                    2002
_chemical_formula_moiety         '2(H15 N5 Na +), (As4 2-), 3 (H3 N)'
_chemical_formula_sum            'As4 H39 N13 Na2'
_chemical_formula_weight         567.06
_chemical_name_systematic
'Bis (pentammin sodium) tetraarsenide-ammonia (1/3)'
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 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                 98.59(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.042(1)
_cell_length_b                   12.287(1)
_cell_length_c                   16.122(1)
_cell_measurement_reflns_used    2211
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      25.90
_cell_measurement_theta_min      2.09
_cell_volume                     2358.7(3)
_computing_cell_refinement       IPDS
_computing_data_collection       'IPDS (Stoe & Cie, 1998)'
_computing_data_reduction        IPDS
_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 0.962
_diffrn_measured_fraction_theta_max 0.962
_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  0.0677
_diffrn_reflns_av_sigmaI/netI    0.0489
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16220
_diffrn_reflns_theta_full        25.90
_diffrn_reflns_theta_max         25.90
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    5.662
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.588
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1124
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.585
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.885
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     106
_refine_ls_number_reflns         2211
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.885
_refine_ls_R_factor_all          0.0746
_refine_ls_R_factor_gt           0.0332
_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^)+(0.0349P)^2^+0.0000P] where P==(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0646
_refine_ls_wR_factor_ref         0.0722
_reflns_number_gt                1230
_reflns_number_total             2211
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b108879c.txt
_cod_data_source_block           '[Na(NH~3~)~5~]~2~[As~4~](NH~3~)~3~'
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_original_formula_sum        'H39 As4 N13 Na2'
_cod_database_code               7114544