#------------------------------------------------------------------------------
#$Date: 2016-02-14 15:26:36 +0100 (dom 14 de feb de 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100973.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100973
loop_
_publ_author_name
'David B. Mitzi'
_publ_contact_author_address
;IBM T. J. Watson Research Center
P.O. Box 218
Yorktown Heights, NY  10598
;
_publ_contact_author_email       dmitzi@us.ibm.com
_publ_contact_author_fax         914-945-2141
_publ_contact_author_name        'Dr. David B. Mitzi'
_publ_contact_author_phone       914-945-4176
_publ_section_title
;
Synthesis, Structure, and Thermal Properties of Soluble Hydrazinium
Germanium(IV) and Tin(IV) Selenide Salts
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3755
_journal_page_last               3761
_journal_paper_doi               10.1021/ic048276l
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         'N8 H20 Ge2 Se6'
_chemical_formula_sum            'Ge2 H20 N8 Se6'
_chemical_formula_weight         751.14
_chemical_name_common            'hydrazinium germanium(IV) selenide'
_chemical_name_systematic        'hydrazinium germanium(IV) selenide'
_space_group_IT_number           110
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      110
_symmetry_space_group_name_Hall  'I 4bw -2c'
_symmetry_space_group_name_H-M   'I 41 c d'
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_formula_units_Z            8
_cell_length_a                   12.7080(12)
_cell_length_b                   12.7080(12)
_cell_length_c                   21.9553(20)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      20.00
_cell_volume                     3545.6(6)
_computing_data_reduction        'NRCVAX DATRD2'
_computing_molecular_graphics    NRCVAX
_computing_publication_material  'NRCVAX TABLES Jan 94 Version'
_computing_structure_refinement  'NRCVAX LSTSQ'
_computing_structure_solution    'NRCVAX SOLVER'
_diffrn_ambient_temperature      293
_diffrn_measurement_device       'SMART 1000'
_diffrn_measurement_method       CCD
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Molybdenum K\a'
_diffrn_radiation_wavelength     0.70930
_diffrn_reflns_av_R_equivalents  0.025
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -3
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            17454
_diffrn_reflns_theta_max         27.44
_diffrn_reflns_theta_min         0.00
_diffrn_source                   'xray tube'
_diffrn_source_type              'Bruker SMART 1000'
_exptl_absorpt_coefficient_mu    15.70
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    2.814
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             2754.72
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.53
_refine_diff_density_min         -0.39
_refine_ls_abs_structure_Flack   -.016(83)
_refine_ls_extinction_coef       922(137)
_refine_ls_extinction_method     Larson
_refine_ls_goodness_of_fit_obs   0.98
_refine_ls_matrix_type           full
_refine_ls_number_parameters     115
_refine_ls_number_reflns         880
_refine_ls_R_factor_all          0.019
_refine_ls_R_factor_obs          0.019
_refine_ls_shift/esd_max         0.000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'calc w=1/(σ²(F)+0.0003F²)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.027
_refine_ls_wR_factor_obs         0.027
_reflns_number_observed          1726
_reflns_number_total             2031
_reflns_observed_criterion       'Inet > 2.0\s(Inet)'
_cod_data_source_file            ic048276lsi20050307_015625_2.cif
_cod_data_source_block           hydgese
_cod_original_cell_volume        3545.6(5)
_cod_original_formula_sum        'N8 H20 Ge2 Se6'
_cod_database_code               1100973
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
1/2+x,1/2+y,1/2+z
-y,1/2+x,1/4+z
1/2-y,x,3/4+z
1/2-x,1/2-y,1/2+z
-x,-y,z
1/2+y,-x,3/4+z
y,1/2-x,1/4+z
-x,y,1/2+z
1/2-x,1/2+y,z
y,1/2+x,3/4+z
1/2+y,x,1/4+z
1/2+x,1/2-y,z
x,-y,1/2+z
1/2-y,-x,1/4+z
-y,1/2-x,3/4+z
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
_atom_site_aniso_type_symbol
Se1 0.02346(23) 0.0315(3) 0.0240(3) 0.00061(19) 0.0011(8) 0.0014(7) Se
Se2 0.0446(6) 0.0294(6) 0.0252(7) -0.0006(3) -0.0020(10) -0.0046(6) Se
Ge1 0.0263(11) 0.0235(11) 0.0212(13) 0.0016(3) 0.00000 0.00000 Ge
Se3 0.0423(7) 0.0323(7) 0.0287(8) 0.0018(3) 0.0003(8) -0.0098(6) Se
Ge2 0.0321(12) 0.0257(11) 0.0139(12) 0.0000(3) 0.00000 0.00000 Ge
N1 0.038(3) 0.036(3) 0.047(4) 0.0018(22) -0.002(5) -0.002(4) N
N3 0.046(3) 0.043(3) 0.053(4) -0.0045(25) 0.011(6) 0.002(4) N
N2 0.044(3) 0.034(3) 0.037(3) -0.0005(23) -0.006(4) 0.004(3) N
N4 0.041(4) 0.032(3) 0.059(4) -0.003(3) 0.003(3) -0.002(3) N
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_type_symbol
Se1 0.35986(4) 0.00673(5) 0.13547 0.0263(5) Uani . . Se
Se2 0.49018(8) -0.15314(11) 0.00474(13) 0.0330(6) Uani . . Se
Ge1 0.50000 0.00000 0.20966(22) 0.0236(11) Uani . S Ge
Se3 0.50708(7) 0.15495(13) 0.26500(13) 0.0345(7) Uani . . Se
Ge2 0.50000 0.00000 0.06067(21) 0.0239(12) Uani . S Ge
N1 0.3919(4) 0.7259(4) 0.1332(7) 0.040(3) Uani . . N
N3 0.8493(4) 0.2061(5) 0.1356(7) 0.047(4) Uani . . N
N2 0.4430(5) 0.6242(4) 0.1372(6) 0.038(3) Uani . . N
N4 0.8055(5) 0.2306(6) 0.0772(5) 0.044(4) Uani . . N
H1 0.727(7) 0.269(7) 0.086(4) 0.07(3) Uiso . . H
H2 0.415(8) 0.581(8) 0.167(5) 0.09(3) Uiso . . H
H3 0.804(9) 0.154(9) 0.151(6) 0.16(5) Uiso . . H
H4 0.421(7) 0.587(7) 0.105(4) 0.07(3) Uiso . . H
H5 0.394(8) 0.753(7) 0.166(4) 0.08(4) Uiso . . H
H6 0.856(6) 0.274(7) 0.152(4) 0.07(3) Uiso . . H
H7 0.851(7) 0.272(8) 0.062(4) 0.07(3) Uiso . . H
H8 0.431(6) 0.760(5) 0.099(3) 0.054(22) Uiso . . H
H9 0.800(5) 0.177(6) 0.060(3) 0.040(22) Uiso . . H
H10 0.526(11) 0.646(11) 0.161(7) 0.18(7) Uiso . . H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
N ? 0.006 0.003 'International Tables Vol. IV Table 2.2B'
H ? 0.000 0.000 'International Tables Vol. IV Table 2.2B'
Ge ? 0.155 1.800 'International Tables Vol. IV Table 2.2B'
Se ? -0.093 2.226 'International Tables Vol. IV Table 2.2B'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
? ? ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
Ge1 Se1 Ge2 85.06(12)
Se1 Ge1 Se1a 95.17(17)
Se1 Ge1 Se3 110.64(5)
Se1 Ge1 Se3a 110.82(5)
Se1a Ge1 Se3 110.82(5)
Se1a Ge1 Se3a 110.64(5)
Se3 Ge1 Se3a 116.71(22)
Se1 Ge2 Se1a 94.71(16)
Se1 Ge2 Se2 110.55(5)
Se1 Ge2 Se2a 111.78(5)
Se1a Ge2 Se2 111.78(5)
Se1a Ge2 Se2a 110.55(5)
Se2 Ge2 Se2a 115.60(21)
N2 N1 H5 108(7)
N2 N1 H8 102(4)
H5 N1 H8 118(8)
N4 N3 H3 103(8)
N4 N3 H6 100(5)
H3 N3 H6 124(9)
N1 N2 H2 113(6)
N1 N2 H4 106(6)
N1 N2 H10 102(7)
H2 N2 H4 97(8)
H2 N2 H10 99(9)
H4 N2 H10 137(9)
N3 N4 H1 105(5)
N3 N4 H7 102(6)
N3 N4 H9 106(5)
H1 N4 H7 113(7)
H1 N4 H9 112(7)
H7 N4 H9 114(8)
N2 H2 H4 40(6)
N2 H4 H2 41(6)
N1 H5 H8 34(5)
N4 H7 H9 31(5)
N1 H8 H5 27(4)
N4 H9 H7 34(5)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Se1 Ge1 2.415(3)
Se1 Ge2 2.424(3)
Se2 Ge2 2.305(3)
Ge1 Se1a 2.415(3)
Ge1 Se3 2.316(3)
Ge1 Se3a 2.316(3)
Ge2 Se1a 2.424(3)
Ge2 Se2a 2.305(3)
N1 N2 1.450(7)
N1 H5 0.80(9)
N1 H8 1.01(8)
N3 N4 1.433(17)
N3 H3 0.94(13)
N3 H6 0.94(9)
N2 H2 0.93(11)
N2 H4 0.90(9)
N2 H10 1.21(13)
N4 H1 1.12(9)
N4 H7 0.85(10)
N4 H9 0.79(7)
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?
