#------------------------------------------------------------------------------
#$Date: 2018-11-01 06:09:45 +0200 (Thu, 01 Nov 2018) $
#$Revision: 211748 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/01/1550169.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_1550169
loop_
_publ_author_name
'Giltzau, Niels Ole'
'Köckerling, Martin'
_publ_section_title
;
 Bis(tetramethylguanidinium) hexachloridotellurate(IV)
;
_journal_coeditor_code           XI4001
_journal_issue                   10
_journal_name_full               IUCrData
_journal_page_first              x181488
_journal_paper_doi               10.1107/S2414314618014888
_journal_volume                  3
_journal_year                    2018
_chemical_formula_iupac          '2C5 H14 N3 +, Cl6 Te 2-'
_chemical_formula_moiety         '2(C5 H14 N3 +), (Cl6 Te 2-)'
_chemical_formula_sum            'C10 H28 Cl6 N6 Te'
_chemical_formula_weight         572.68
_chemical_melting_point          407
_chemical_name_systematic
;
Bis(tetramethylguanidinium) hexachloridotellurate(IV)
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_Hall           '-F 2uv 2vw'
_space_group_name_H-M_alt        'F d d d'
_symmetry_space_group_name_Hall  '-F 2uv 2vw'
_symmetry_space_group_name_H-M   'F d d d :2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'form.cif (version 2.0)'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   7.3899(5)
_cell_length_b                   22.447(2)
_cell_length_c                   28.512(2)
_cell_measurement_reflns_used    9942
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      32.5345
_cell_measurement_theta_min      2.309
_cell_volume                     4729.6(6)
_computing_cell_refinement
;
SAINT (Bruker, 2017)
;
_computing_data_collection
;
APEX3 (Bruker, 2017)
;
_computing_data_reduction
;
SAINT (Bruker, 2017)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg & Putz, 2014)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS2014 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0272
_diffrn_reflns_av_unetI/netI     0.0080
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            47585
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         32.563
_diffrn_reflns_theta_min         2.858
_exptl_absorpt_coefficient_mu    1.916
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2017)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_density_method    none
_exptl_crystal_description       stick
_exptl_crystal_F_000             2272
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.388
_refine_diff_density_min         -0.374
_refine_ls_extinction_coef       0.000156(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2014 (Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref   1.256
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     62
_refine_ls_number_reflns         2158
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.256
_refine_ls_R_factor_all          0.0142
_refine_ls_R_factor_gt           0.0128
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0103P)²+6.2116P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0333
_refine_ls_wR_factor_ref         0.0342
_reflns_number_gt                2057
_reflns_number_total             2158
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            xi4001sup1.cif
_cod_data_source_block           I
_cod_database_code               1550169
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop  which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.479
_shelx_estimated_absorpt_t_max   0.803
_shelxl_version_number           201.4
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+3/4, -y+3/4, z'
'-x+3/4, y, -z+3/4'
'x, -y+3/4, -z+3/4'
'x, y+1/2, z+1/2'
'-x+3/4, -y+5/4, z+1/2'
'-x+3/4, y+1/2, -z+5/4'
'x, -y+5/4, -z+5/4'
'x+1/2, y, z+1/2'
'-x+5/4, -y+3/4, z+1/2'
'-x+5/4, y, -z+5/4'
'x+1/2, -y+3/4, -z+5/4'
'x+1/2, y+1/2, z'
'-x+5/4, -y+5/4, z'
'-x+5/4, y+1/2, -z+3/4'
'x+1/2, -y+5/4, -z+3/4'
'-x, -y, -z'
'x-3/4, y-3/4, -z'
'x-3/4, -y, z-3/4'
'-x, y-3/4, z-3/4'
'-x, -y+1/2, -z+1/2'
'x-3/4, y-1/4, -z+1/2'
'x-3/4, -y+1/2, z-1/4'
'-x, y-1/4, z-1/4'
'-x+1/2, -y, -z+1/2'
'x-1/4, y-3/4, -z+1/2'
'x-1/4, -y, z-1/4'
'-x+1/2, y-3/4, z-1/4'
'-x+1/2, -y+1/2, -z'
'x-1/4, y-1/4, -z'
'x-1/4, -y+1/2, z-3/4'
'-x+1/2, y-1/4, z-3/4'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
Te Te1 0.8750 0.3750 0.3750 0.01545(4) Uani d 1
Cl Cl1 0.8750 0.3750 0.46396(2) 0.02182(6) Uani d 1
Cl Cl2 0.63226(3) 0.45506(2) 0.37388(2) 0.02254(5) Uani d 1
N N1 0.3750 0.3750 0.45159(4) 0.0222(2) Uani d 1
H H1 0.447(2) 0.3533(6) 0.4372(5) 0.030(4) Uiso d 1
C C1 0.3750 0.3750 0.49798(5) 0.0184(2) Uani d 1
N N2 0.30040(10) 0.42051(4) 0.52161(3) 0.0241(2) Uani d 1
C C2 0.1980(2) 0.41017(6) 0.56481(4) 0.0381(3) Uani d 1
H H2A 0.0721 0.4226 0.5602 0.057 Uiso calc 1
H H2B 0.2517 0.4333 0.5904 0.057 Uiso calc 1
H H2C 0.2017 0.3677 0.5727 0.057 Uiso calc 1
C C3 0.2619(2) 0.47675(5) 0.49795(4) 0.0307(2) Uani d 1
H H3A 0.3543 0.4842 0.4740 0.046 Uiso calc 1
H H3B 0.2629 0.5092 0.5209 0.046 Uiso calc 1
H H3C 0.1426 0.4746 0.4831 0.046 Uiso calc 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1507 0.1611 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0066 0.0034 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Te Te -0.4979 1.7022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cl1 Te1 Cl1 . 3_655 180.0 y
Cl1 Te1 Cl2 . 4 89.282(5) y
Cl1 Te1 Cl2 3_655 4 90.718(5) n
Cl1 Te1 Cl2 . . 90.718(5) y
Cl1 Te1 Cl2 3_655 . 89.282(5) n
Cl2 Te1 Cl2 4 . 90.120(10) y
Cl1 Te1 Cl2 . 3_655 89.283(5) n
Cl1 Te1 Cl2 3_655 3_655 90.717(5) n
Cl2 Te1 Cl2 4 3_655 178.570(10) y
Cl2 Te1 Cl2 . 3_655 89.900(10) n
Cl1 Te1 Cl2 . 2_655 90.717(5) y
Cl1 Te1 Cl2 3_655 2_655 89.283(5) n
Cl2 Te1 Cl2 4 2_655 89.900(10) y
Cl2 Te1 Cl2 . 2_655 178.570(10) n
Cl2 Te1 Cl2 3_655 2_655 90.120(10) n
C1 N1 H1 . . 120.0(10) n
N1 C1 N2 . 2 120.14(6) y
N1 C1 N2 . . 120.14(6) n
N2 C1 N2 2 . 119.70(10) y
C1 N2 C3 . . 120.43(9) y
C1 N2 C2 . . 120.93(9) y
C3 N2 C2 . . 115.15(9) y
N2 C2 H2A . . 109.5 y
N2 C2 H2B . . 109.5 n
H2A C2 H2B . . 109.5 n
N2 C2 H2C . . 109.5 n
H2A C2 H2C . . 109.5 n
H2B C2 H2C . . 109.5 n
N2 C3 H3A . . 109.5 n
N2 C3 H3B . . 109.5 n
H3A C3 H3B . . 109.5 n
N2 C3 H3C . . 109.5 n
H3A C3 H3C . . 109.5 n
H3B C3 H3C . . 109.5 n
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Te1 Cl1 . 2.5363(4) y
Te1 Cl1 3_655 2.5364(4) n
Te1 Cl2 4 2.5394(3) n
Te1 Cl2 . 2.5394(3) y
Te1 Cl2 3_655 2.5394(3) n
Te1 Cl2 2_655 2.5394(3) n
N1 C1 . 1.323(2) y
N1 H1 . 0.83(2) n
C1 N2 2 1.3420(10) n
C1 N2 . 1.3420(10) y
N2 C3 . 1.4590(10) y
N2 C2 . 1.464(2) y
C2 H2A . 0.9800 n
C2 H2B . 0.9800 n
C2 H2C . 0.9800 n
C3 H3A . 0.9800 n
C3 H3B . 0.9800 n
C3 H3C . 0.9800 n
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N1 H1 Cl2 4 0.83(2) 2.57(2) 3.3875(8) 167.0(10)
C2 H2B Cl2 17_666 0.98 2.84 3.7120(10) 149.1
C3 H3B Cl1 17_666 0.98 2.82 3.6440(10) 141.6

_cod_database_fobs_code 1550169
