#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/01/4300115.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_4300115
loop_
_publ_author_name
'Xiaobing Xie'
'Timothy Hughbanks'
_publ_section_title
;
Reduced Zirconium Halide Clusters in Aqueous Solution
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              555
_journal_page_last               561
_journal_paper_doi               10.1021/ic9908423
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'B Cl18 H52.5 O24 Rb0.44 Zr6'
_chemical_formula_weight         1670.76
_space_group_IT_number           229
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-I 4 2 3'
_symmetry_space_group_name_H-M   'I m -3 m'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.8962(3)
_cell_length_b                   13.8962(3)
_cell_length_c                   13.8962(3)
_cell_measurement_temperature    213(2)
_cell_volume                     2683.42(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_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  0.0607
_diffrn_reflns_av_sigmaI/netI    0.0256
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6361
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.07
_exptl_absorpt_coefficient_mu    2.472
_exptl_absorpt_correction_T_max  0.8864
_exptl_absorpt_correction_T_min  0.7901
_exptl_crystal_density_diffrn    2.068
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1624
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.442
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.093
_refine_ls_extinction_coef       0.00068(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     22
_refine_ls_number_reflns         337
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0264
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0351P)²+1.8503P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0646
_refine_ls_wR_factor_ref         0.0669
_reflns_number_gt                252
_reflns_number_total             337
_reflns_threshold_expression     >2sigma(I)
_cod_original_formula_sum        'H52.50 B Cl18 O24 Rb0.44 Zr6'
_cod_database_code               4300115
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y, x, -z'
'-y, -x, -z'
'y, -x, z'
'-y, x, z'
'x, z, -y'
'-x, z, y'
'-x, -z, -y'
'x, -z, y'
'z, y, -x'
'z, -y, x'
'-z, y, x'
'-z, -y, -x'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'z+1/2, -x+1/2, -y+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-z+1/2, x+1/2, -y+1/2'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x+1/2'
'-y+1/2, -z+1/2, x+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'x+1/2, z+1/2, -y+1/2'
'-x+1/2, z+1/2, y+1/2'
'-x+1/2, -z+1/2, -y+1/2'
'x+1/2, -z+1/2, y+1/2'
'z+1/2, y+1/2, -x+1/2'
'z+1/2, -y+1/2, x+1/2'
'-z+1/2, y+1/2, x+1/2'
'-z+1/2, -y+1/2, -x+1/2'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-z, -x, -y'
'-z, x, y'
'z, x, -y'
'z, -x, y'
'-y, -z, -x'
'y, -z, x'
'-y, z, x'
'y, z, -x'
'-y, -x, z'
'y, x, z'
'-y, x, -z'
'y, -x, -z'
'-x, -z, y'
'x, -z, -y'
'x, z, y'
'-x, z, -y'
'-z, -y, x'
'-z, y, -x'
'z, -y, -x'
'z, y, x'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'-z+1/2, -x+1/2, -y+1/2'
'-z+1/2, x+1/2, y+1/2'
'z+1/2, x+1/2, -y+1/2'
'z+1/2, -x+1/2, y+1/2'
'-y+1/2, -z+1/2, -x+1/2'
'y+1/2, -z+1/2, x+1/2'
'-y+1/2, z+1/2, x+1/2'
'y+1/2, z+1/2, -x+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-x+1/2, -z+1/2, y+1/2'
'x+1/2, -z+1/2, -y+1/2'
'x+1/2, z+1/2, y+1/2'
'-x+1/2, z+1/2, -y+1/2'
'-z+1/2, -y+1/2, x+1/2'
'-z+1/2, y+1/2, -x+1/2'
'z+1/2, -y+1/2, -x+1/2'
'z+1/2, y+1/2, x+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr1 Zr 0.0000 0.16582(5) 0.0000 0.0174(3) Uani 1 8 d S . .
B B 0.0000 0.0000 0.0000 0.016(4) Uani 1 48 d S . .
Cl1 Cl 0.18315(6) 0.18315(6) 0.0000 0.0256(4) Uani 1 4 d S . .
Cl2 Cl 0.0000 0.35698(15) 0.0000 0.0380(5) Uani 1 8 d S . .
O1 O 0.15981(19) 0.3996(2) 0.15981(19) 0.0766(13) Uani 1 2 d S . .
Rb Rb 0.2500 0.2500 0.2500 0.057(4) Uani 0.108(4) 12 d SP . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B 0.0013 0.0007 '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'
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'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rb Rb -0.9393 2.9676 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
B Zr1 Cl1 95.41(2) . 5 ?
B Zr1 Cl1 95.41(2) . . ?
Cl1 Zr1 Cl1 89.491(5) 5 . ?
B Zr1 Cl1 95.41(2) . 55 ?
Cl1 Zr1 Cl1 169.19(5) 5 55 ?
Cl1 Zr1 Cl1 89.491(5) . 55 ?
B Zr1 Cl1 95.41(2) . 3 ?
Cl1 Zr1 Cl1 89.491(5) 5 3 ?
Cl1 Zr1 Cl1 169.19(5) . 3 ?
Cl1 Zr1 Cl1 89.491(5) 55 3 ?
B Zr1 Cl2 180.0 . . ?
Cl1 Zr1 Cl2 84.59(2) 5 . ?
Cl1 Zr1 Cl2 84.59(2) . . ?
Cl1 Zr1 Cl2 84.59(2) 55 . ?
Cl1 Zr1 Cl2 84.59(2) 3 . ?
B Zr1 Zr1 45.0 . 53 ?
Cl1 Zr1 Zr1 140.41(2) 5 53 ?
Cl1 Zr1 Zr1 93.820(18) . 53 ?
Cl1 Zr1 Zr1 50.41(2) 55 53 ?
Cl1 Zr1 Zr1 93.820(18) 3 53 ?
Cl2 Zr1 Zr1 135.0 . 53 ?
B Zr1 Zr1 45.0 . 57 ?
Cl1 Zr1 Zr1 93.820(18) 5 57 ?
Cl1 Zr1 Zr1 140.41(2) . 57 ?
Cl1 Zr1 Zr1 93.820(18) 55 57 ?
Cl1 Zr1 Zr1 50.41(2) 3 57 ?
Cl2 Zr1 Zr1 135.0 . 57 ?
Zr1 Zr1 Zr1 60.0 53 57 ?
B Zr1 Zr1 45.0 . 5 ?
Cl1 Zr1 Zr1 50.41(2) 5 5 ?
Cl1 Zr1 Zr1 93.820(18) . 5 ?
Cl1 Zr1 Zr1 140.41(2) 55 5 ?
Cl1 Zr1 Zr1 93.820(18) 3 5 ?
Cl2 Zr1 Zr1 135.0 . 5 ?
Zr1 Zr1 Zr1 90.0 53 5 ?
Zr1 Zr1 Zr1 60.0 57 5 ?
B Zr1 Zr1 45.0 . 9 ?
Cl1 Zr1 Zr1 93.820(18) 5 9 ?
Cl1 Zr1 Zr1 50.41(2) . 9 ?
Cl1 Zr1 Zr1 93.820(18) 55 9 ?
Cl1 Zr1 Zr1 140.41(2) 3 9 ?
Cl2 Zr1 Zr1 135.0 . 9 ?
Zr1 Zr1 Zr1 60.0 53 9 ?
Zr1 Zr1 Zr1 90.0 57 9 ?
Zr1 Zr1 Zr1 60.0 5 9 ?
Zr1 B Zr1 180.0 57 9 ?
Zr1 B Zr1 90.0 57 49 ?
Zr1 B Zr1 90.0 9 49 ?
Zr1 B Zr1 90.0 57 5 ?
Zr1 B Zr1 90.0 9 5 ?
Zr1 B Zr1 90.0 49 5 ?
Zr1 B Zr1 90.0 57 53 ?
Zr1 B Zr1 90.0 9 53 ?
Zr1 B Zr1 90.0 49 53 ?
Zr1 B Zr1 180.0 5 53 ?
Zr1 B Zr1 90.0 57 . ?
Zr1 B Zr1 90.0 9 . ?
Zr1 B Zr1 180.0 49 . ?
Zr1 B Zr1 90.0 5 . ?
Zr1 B Zr1 90.0 53 . ?
Zr1 Cl1 Zr1 79.19(5) . 9 ?
Zr1 Cl1 Rb 105.816(10) . . ?
Zr1 Cl1 Rb 105.816(10) 9 . ?
Zr1 Cl1 Rb 105.816(10) . 26_554 ?
Zr1 Cl1 Rb 105.816(10) 9 26_554 ?
Rb Cl1 Rb 138.57(4) . 26_554 ?
Zr1 Cl2 O1 100.68(7) . . ?
Rb O1 O1 59.597(11) . 81 ?
Rb O1 O1 59.597(11) . 77 ?
O1 O1 O1 116.89(8) 81 77 ?
Rb O1 O1 139.55(7) . 51_565 ?
O1 O1 O1 107.38(9) 81 51_565 ?
O1 O1 O1 107.38(9) 77 51_565 ?
Rb O1 Cl2 119.76(11) . . ?
O1 O1 Cl2 111.53(14) 81 . ?
O1 O1 Cl2 111.53(14) 77 . ?
O1 O1 Cl2 100.68(7) 51_565 . ?
O1 Rb O1 180.0 81 9 ?
O1 Rb O1 119.19(2) 81 77 ?
O1 Rb O1 60.81(2) 9 77 ?
O1 Rb O1 60.81(2) 81 5 ?
O1 Rb O1 119.19(2) 9 5 ?
O1 Rb O1 180.00(10) 77 5 ?
O1 Rb O1 119.19(2) 81 73 ?
O1 Rb O1 60.81(2) 9 73 ?
O1 Rb O1 119.19(2) 77 73 ?
O1 Rb O1 60.81(2) 5 73 ?
O1 Rb O1 60.81(2) 81 . ?
O1 Rb O1 119.19(2) 9 . ?
O1 Rb O1 60.81(2) 77 . ?
O1 Rb O1 119.19(2) 5 . ?
O1 Rb O1 180.00(10) 73 . ?
O1 Rb Cl1 110.70(6) 81 . ?
O1 Rb Cl1 69.30(6) 9 . ?
O1 Rb Cl1 61.16(7) 77 . ?
O1 Rb Cl1 118.84(8) 5 . ?
O1 Rb Cl1 110.70(6) 73 . ?
O1 Rb Cl1 69.30(6) . . ?
O1 Rb Cl1 69.30(6) 81 81 ?
O1 Rb Cl1 110.70(6) 9 81 ?
O1 Rb Cl1 69.30(6) 77 81 ?
O1 Rb Cl1 110.70(6) 5 81 ?
O1 Rb Cl1 118.84(7) 73 81 ?
O1 Rb Cl1 61.16(7) . 81 ?
Cl1 Rb Cl1 122.03(3) . 81 ?
O1 Rb Cl1 118.84(7) 81 77 ?
O1 Rb Cl1 61.16(7) 9 77 ?
O1 Rb Cl1 69.30(6) 77 77 ?
O1 Rb Cl1 110.70(6) 5 77 ?
O1 Rb Cl1 69.30(6) 73 77 ?
O1 Rb Cl1 110.70(6) . 77 ?
Cl1 Rb Cl1 122.03(3) . 77 ?
Cl1 Rb Cl1 57.97(3) 81 77 ?
O1 Rb Cl1 61.16(7) 81 5 ?
O1 Rb Cl1 118.84(7) 9 5 ?
O1 Rb Cl1 110.70(6) 77 5 ?
O1 Rb Cl1 69.30(6) 5 5 ?
O1 Rb Cl1 110.70(6) 73 5 ?
O1 Rb Cl1 69.30(6) . 5 ?
Cl1 Rb Cl1 57.97(3) . 5 ?
Cl1 Rb Cl1 122.03(3) 81 5 ?
Cl1 Rb Cl1 180.0 77 5 ?
O1 Rb Cl1 69.30(6) 81 73 ?
O1 Rb Cl1 110.70(6) 9 73 ?
O1 Rb Cl1 118.84(7) 77 73 ?
O1 Rb Cl1 61.16(8) 5 73 ?
O1 Rb Cl1 69.30(6) 73 73 ?
O1 Rb Cl1 110.70(6) . 73 ?
Cl1 Rb Cl1 180.0 . 73 ?
Cl1 Rb Cl1 57.97(3) 81 73 ?
Cl1 Rb Cl1 57.97(3) 77 73 ?
Cl1 Rb Cl1 122.03(3) 5 73 ?
O1 Rb Cl1 110.70(6) 81 9 ?
O1 Rb Cl1 69.30(6) 9 9 ?
O1 Rb Cl1 110.70(6) 77 9 ?
O1 Rb Cl1 69.30(6) 5 9 ?
O1 Rb Cl1 61.16(7) 73 9 ?
O1 Rb Cl1 118.84(7) . 9 ?
Cl1 Rb Cl1 57.97(3) . 9 ?
Cl1 Rb Cl1 180.0 81 9 ?
Cl1 Rb Cl1 122.03(3) 77 9 ?
Cl1 Rb Cl1 57.97(3) 5 9 ?
Cl1 Rb Cl1 122.03(3) 73 9 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zr1 B 2.3042(7) . ?
Zr1 Cl1 2.5565(10) 5 ?
Zr1 Cl1 2.5565(10) . ?
Zr1 Cl1 2.5565(10) 55 ?
Zr1 Cl1 2.5565(10) 3 ?
Zr1 Cl2 2.656(2) . ?
Zr1 Zr1 3.2587(10) 53 ?
Zr1 Zr1 3.2587(10) 57 ?
Zr1 Zr1 3.2587(10) 5 ?
Zr1 Zr1 3.2587(10) 9 ?
B Zr1 2.3042(7) 57 ?
B Zr1 2.3042(7) 9 ?
B Zr1 2.3042(7) 49 ?
B Zr1 2.3042(7) 5 ?
B Zr1 2.3042(7) 53 ?
Cl1 Zr1 2.5565(10) 9 ?
Cl1 Rb 3.7141(5) . ?
Cl1 Rb 3.7141(5) 26_554 ?
Cl2 O1 3.196(4) . ?
O1 Rb 2.732(4) . ?
O1 O1 2.765(4) 81 ?
O1 O1 2.765(4) 77 ?
O1 O1 2.790(7) 51_565 ?
Rb O1 2.732(4) 81 ?
Rb O1 2.732(4) 9 ?
Rb O1 2.732(4) 77 ?
Rb O1 2.732(4) 5 ?
Rb O1 2.732(4) 73 ?
Rb Cl1 3.7141(5) 81 ?
Rb Cl1 3.7141(5) 77 ?
Rb Cl1 3.7141(5) 5 ?
Rb Cl1 3.7141(5) 73 ?
Rb Cl1 3.7141(5) 9 ?
