##############################################################################
#                                                                            #
# This CIF contains the data for a data article accepted for                 #
# publication in IUCrData. It conforms to the requirements of                #
# Notes for Authors for IUCrData, and has been                               #
# peer reviewed under the auspices of IUCrData.                              #
#                                                                            #
# Full details of the Crystallographic Information File format               #
# are given in the paper "The Crystallographic Information File (CIF):       #
# a New Standard Archive File for Crystallography" by S. R. Hall, F. H.      #
# Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685].                  #
#                                                                            #
# The current version of the core CIF dictionary is obtainable from          #
# ftp://ftp.iucr.org/pub/cif_core.dic.                                       #
#                                                                            #
# Software is freely available for graphical display of the structure(s)     #
# in this CIF. For information consult the CIF software page                 #
# http://www.iucr.org/resources/cif/software.                                #
#                                                                            #
# This file may be used for bona fide research purposes within the           #
# scientific community so long as proper attribution is given to the data    # 
# article from which it was obtained.                                        #
#                                                                            #
##############################################################################
data_I
_audit_creation_method     'ciftab-2016 (M. Köckerling, 2016)'
_journal_date_recd_electronic     2021-06-01
_journal_date_accepted     2021-07-06
_journal_name_full     'IUCrData'
_journal_year     2021
_journal_volume     6
_journal_issue      7
_journal_page_first     0
_journal_page_last     0
_journal_paper_category     HI
_journal_paper_doi     10.1107/S2414314621006969
_journal_coeditor_code     BT4115
_publ_contact_author_name     'Köckerling, Martin'
_publ_contact_author_address
;
Universität Rostock
Institut für Chemie
Anorganische Festkörperchemie
Albert-Einstein-Str. 3a
D-18059 Rostock
Germany
;
_publ_contact_author_email     'Martin.Koeckerling@uni-rostock.de'
_publ_contact_author_fax     '++49 381 498 6382'
_publ_contact_author_phone     '++49 381 498 6390'
_publ_section_title
;
Hexaaquadodeca-μ₂-chlorido-octahedro-hexaniobium diiodide
;
loop_
    _publ_author_name
    _publ_author_address
    'Schröder, Florian'
;
Universität Rostock
Institut für Chemie
Anorganische Festkörperchemie
Albert-Einstein-Str. 3a
D-18059 Rostock
Germany
;
    'Köckerling, Martin'
;
Universität Rostock
Institut für Chemie
Anorganische Festkörperchemie
Albert-Einstein-Str. 3a
D-18059 Rostock
Germany
;
_publ_section_synopsis
;
The crystal structure of the cluster complex [Nb₆Cl₁₂(H₂O)₆]I₂ is
described. The octahedral Nb₆ cluster core is coordinated by twelve chlorido
and six water ligands. The two iodide ions are not bonded to the cluster unit
but are present in the crystal structure as the counter-anion to the cluster
cation.
;
_chemical_name_systematic
;
Hexaaquadodeca-μ₂-chlorido-octahedro-hexaniobium diiodide
;
_chemical_formula_moiety     'H12 Cl12 I2 Nb6 O6'
_chemical_formula_sum     'H12 Cl12 I2 Nb6 O6'
_chemical_formula_iupac     '[Nb6 Cl12 (H2 O)6] I2'
_chemical_formula_weight     1344.76
_space_group_crystal_system     trigonal
_space_group_name_H-M_alt     'P -3 1 m'
_space_group_name_Hall     '-P 3 2'
loop_
    _space_group_symop_operation_xyz
    'x, y, z'
    '-y, x-y, z'
    '-x+y, -x, z'
    '-y, -x, -z'
    'x, x-y, -z'
    '-x+y, y, -z'
    '-x, -y, -z'
    'y, -x+y, -z'
    'x-y, x, -z'
    'y, x, z'
    '-x, -x+y, z'
    'x-y, -y, z'
_cell_length_a     9.3911(8)
_cell_length_b     9.3911(8)
_cell_length_c     8.6576(9)
_cell_angle_alpha     90
_cell_angle_beta     90
_cell_angle_gamma     120
_cell_volume     661.20(10)
_cell_formula_units_Z     1
_cell_measurement_reflns_used     9268
_cell_measurement_theta_min     2.5045
_cell_measurement_theta_max     34.863
_cell_measurement_temperature     123(2)
_exptl_crystal_description     block
_exptl_crystal_colour     black
_exptl_crystal_size_max     0.200
_exptl_crystal_size_mid     0.200
_exptl_crystal_size_min     0.160
_exptl_crystal_density_diffrn     3.377
_exptl_crystal_density_method     'none'
_exptl_crystal_F_000     616
_exptl_absorpt_coefficient_mu     6.076
_exptl_absorpt_correction_type     multi-scan
_exptl_absorpt_process_details
;
(SADABS, Bruker, 2017)
;
_diffrn_ambient_temperature     123(2)
_diffrn_radiation_type     MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source     'microfocus sealed tube'
_diffrn_measurement_device_type     'Bruker APEXII CCD'
_diffrn_measurement_method     'φ and ω scans'
_diffrn_reflns_number     43489
_diffrn_reflns_av_R_equivalents     0.0314
_diffrn_reflns_av_unetI/netI     0.0062
_diffrn_reflns_theta_min     3.437
_diffrn_reflns_theta_max     34.949
_diffrn_reflns_theta_full     25.000
_diffrn_measured_fraction_theta_max     0.998
_diffrn_measured_fraction_theta_full     0.995
_diffrn_reflns_limit_h_min     -15
_diffrn_reflns_limit_h_max     15
_diffrn_reflns_limit_k_min     -15
_diffrn_reflns_limit_k_max     15
_diffrn_reflns_limit_l_min     -13
_diffrn_reflns_limit_l_max     13
_refine_special_details
;
 The H
atom was located in a difference maps, but refined using a riding model with
O---H = 0.85 Å and with U(H) = 1.5 Ueq(O).
;
_reflns_number_total     1059
_reflns_number_gt     1058
_reflns_threshold_expression     'I > 2σ(I)'
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all     0.0131
_refine_ls_R_factor_gt     0.0130
_refine_ls_wR_factor_gt     0.0335
_refine_ls_wR_factor_ref     0.0335
_refine_ls_goodness_of_fit_ref     1.376
_refine_ls_restrained_S_all     1.376
_refine_ls_number_reflns     1059
_refine_ls_number_parameters     27
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment     constr
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details
              'w=1/[σ²(Fo²)+(0.0050P)²+1.1433P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens     difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary     difmap
_refine_ls_shift/su_max     0.000
_refine_ls_shift/su_mean     0.000
_refine_diff_density_max     0.716
_refine_diff_density_min     -0.813
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef     0.0071(3)
_refine_ls_extinction_expression
                                  'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
loop_
    _atom_type_symbol
    _atom_type_description
    _atom_type_scat_dispersion_real
    _atom_type_scat_dispersion_imag
    _atom_type_scat_source
    'H' 'H' 0.0000 0.0000
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'O' 'O' 0.0106 0.0060
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'Cl' 'Cl' 0.1484 0.1585
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'Nb' 'Nb' -2.0727 0.6215
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'I' 'I' -0.4742 1.8119
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_computing_data_collection
;
APEX3 (Bruker, 2017)
;
_computing_cell_refinement
;
SAINT (Bruker, 2017)
;
_computing_data_reduction
;
SAINT (Bruker, 2017)
;
_computing_structure_solution
;
SHELXS2014 (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg & Putz, 2019)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
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
    _atom_site_disorder_assembly
    _atom_site_disorder_group
    Nb Nb1 0.0000 0.17816(2) 0.13652(2) 0.00709(5) Uani d 1 . .
    Cl Cl1 -0.21059(3) 0.21059(3) 0.0000 0.01203(9) Uani d 1 . .
    Cl Cl2 0.21271(6) 0.21271(6) 0.32300(6) 0.01238(9) Uani d 1 . .
    O O1 0.0000 0.3770(2) 0.2816(2) 0.0167(3) Uani d 1 . .
    H H1A 0.0851 0.4473 0.3300 0.025 Uiso d 1 . .
    I I1 0.333333 0.666667 0.5000 0.01368(6) Uani d 1 . .
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
    Nb1 0.00681(8) 0.00640(6) 0.00821(8) 0.00340(4) 0.00 -0.00114(4)
    Cl1 0.01110(10)
                  0.01110(10)
                            0.0173(2) 0.0082(2) -0.00210(10)
                                                           -0.00210(10)
    Cl2 0.0136(2) 0.0136(2) 0.0106(2) 0.0072(2) -0.00440(10)
                                                           -0.00440(10)
    O1 0.0135(7) 0.0154(5) 0.0205(7) 0.0067(3) 0.00 -0.0085(5)
    I1 0.01186(7) 0.01186(7) 0.01730(10)
                                       0.00593(4) 0.00 0.00
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry.  An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
    _geom_bond_atom_site_label_1
    _geom_bond_atom_site_label_2
    _geom_bond_site_symmetry_2
    _geom_bond_distance
    Nb1 O1 . 2.250(2)
    Nb1 Cl1 . 2.4502(4)
    Nb1 Cl1 8 2.4502(4)
    Nb1 Cl2 2 2.4605(4)
    Nb1 Cl2 . 2.4605(4)
    Nb1 Nb1 9 2.8960(4)
    Nb1 Nb1 8 2.8960(4)
    Nb1 Nb1 2 2.8980(4)
    Nb1 Nb1 3 2.8980(4)
    Cl1 Nb1 9 2.4501(4)
    Cl2 Nb1 3 2.4605(4)
    O1 H1A . 0.8500
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
    O1 Nb1 Cl1 . . 80.29(4)
    O1 Nb1 Cl1 . 8 80.28(4)
    Cl1 Nb1 Cl1 . 8 88.699(7)
    O1 Nb1 Cl2 . 2 82.02(4)
    Cl1 Nb1 Cl2 . 2 88.260(10)
    Cl1 Nb1 Cl2 8 2 162.300(10)
    O1 Nb1 Cl2 . . 82.02(4)
    Cl1 Nb1 Cl2 . . 162.300(10)
    Cl1 Nb1 Cl2 8 . 88.260(10)
    Cl2 Nb1 Cl2 2 . 89.35(3)
    O1 Nb1 Nb1 . 9 134.05(4)
    Cl1 Nb1 Nb1 . 9 53.773(8)
    Cl1 Nb1 Nb1 8 9 96.230(10)
    Cl2 Nb1 Nb1 2 9 96.000(10)
    Cl2 Nb1 Nb1 . 9 143.919(8)
    O1 Nb1 Nb1 . 8 134.05(4)
    Cl1 Nb1 Nb1 . 8 96.230(10)
    Cl1 Nb1 Nb1 8 8 53.773(8)
    Cl2 Nb1 Nb1 2 8 143.919(8)
    Cl2 Nb1 Nb1 . 8 96.010(10)
    Nb1 Nb1 Nb1 9 8 60.040(10)
    O1 Nb1 Nb1 . 2 135.94(3)
    Cl1 Nb1 Nb1 . 2 96.180(6)
    Cl1 Nb1 Nb1 8 2 143.773(8)
    Cl2 Nb1 Nb1 2 2 53.922(8)
    Cl2 Nb1 Nb1 . 2 96.560(10)
    Nb1 Nb1 Nb1 9 2 59.977(5)
    Nb1 Nb1 Nb1 8 2 90.0
    O1 Nb1 Nb1 . 3 135.94(3)
    Cl1 Nb1 Nb1 . 3 143.773(8)
    Cl1 Nb1 Nb1 8 3 96.180(6)
    Cl2 Nb1 Nb1 2 3 96.560(10)
    Cl2 Nb1 Nb1 . 3 53.922(8)
    Nb1 Nb1 Nb1 9 3 90.0
    Nb1 Nb1 Nb1 8 3 59.977(5)
    Nb1 Nb1 Nb1 2 3 60.0
    Nb1 Cl1 Nb1 9 . 72.45(2)
    Nb1 Cl2 Nb1 . 3 72.16(2)
    Nb1 O1 H1A . . 122.0
_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     0.376
_shelx_estimated_absorpt_T_max     0.443
_shelxl_version_number      201.4
