#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/08/4330837.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_4330837
loop_
_publ_author_name
'Matthew J. Polinski'
'Shuao Wang'
'Evgeny V. Alekseev'
'Justin N. Cross'
'Wulf Depmeier'
'Thomas E. Albrecht-Schmitt'
_publ_section_title
;
 Effect of pH and Reaction Time on the Structures of Early Lanthanide(III)
 Borate Perchlorates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11541
_journal_page_last               11548
_journal_paper_doi               10.1021/ic301421e
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         La[B8O10(OH)6(H2O)(ClO4)]0.5H2O
_chemical_formula_sum            'B8 Cl La O21.5'
_chemical_formula_weight         604.84
_chemical_name_common            'Lanthanum(III) Octaborate Perchlorate'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.994(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.858(8)
_cell_length_b                   8.243(6)
_cell_length_c                   21.418(16)
_cell_measurement_reflns_used    4040
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.64
_cell_measurement_theta_min      0.96
_cell_volume                     1727(2)
_computing_cell_refinement       'Smart Saint'
_computing_data_collection       Smart
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXP-91 (Sheldrick, 1997)'
_computing_publication_material  'SHELXCIF-97 (Sheldrick, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'BRUKER apex II'
_diffrn_measurement_method       '0.5 wide w/ exposures'
_diffrn_radiation_monochromator  'Quazar Optics'
_diffrn_radiation_source         'Imus microfocused'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0480
_diffrn_reflns_av_sigmaI/netI    0.0380
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            19624
_diffrn_reflns_theta_full        27.64
_diffrn_reflns_theta_max         27.64
_diffrn_reflns_theta_min         0.96
_exptl_absorpt_coefficient_mu    2.739
_exptl_absorpt_correction_T_max  0.986
_exptl_absorpt_correction_T_min  0.819
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   SHELTXPREP
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    2.326
_exptl_crystal_description       Tablet
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.078
_exptl_crystal_size_mid          0.061
_exptl_crystal_size_min          0.005
_refine_diff_density_max         1.782
_refine_diff_density_min         -2.091
_refine_diff_density_rms         0.249
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.188
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     305
_refine_ls_number_reflns         4040
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.188
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0388
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0222P)²+14.2894P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0898
_refine_ls_wR_factor_ref         0.0930
_reflns_number_gt                3562
_reflns_number_total             4040
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301421e_si_002_01.cif
_cod_data_source_block           LaBClO-1
_cod_original_formula_sum        'B8 Cl La O21.50'
_cod_database_code               4330837
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-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
La1 La 1.48628(3) 0.46465(4) 0.700052(13) 0.00621(9) Uani 1 1 d .
Cl1A Cl 1.50819(19) 0.3305(2) 0.87104(8) 0.0162(5) Uani 0.770(5) 1 d P
Cl1B Cl 1.6107(6) 0.3847(8) 0.8741(3) 0.0183(18) Uani 0.230(5) 1 d P
O12 O 1.2372(3) 0.4727(4) 0.72655(16) 0.0077(7) Uani 1 1 d .
O11 O 1.7499(3) 0.4732(4) 0.72572(16) 0.0077(7) Uani 1 1 d .
O10 O 1.3737(3) 0.1763(4) 0.71900(17) 0.0088(7) Uani 1 1 d .
O9 O 1.3215(4) 0.3749(5) 0.60381(18) 0.0151(8) Uani 1 1 d .
O8 O 1.6096(4) 0.1800(4) 0.72206(17) 0.0091(7) Uani 1 1 d .
O7 O 1.3536(3) 0.7094(4) 0.75172(17) 0.0075(7) Uani 1 1 d .
O6 O 1.6481(4) 0.7121(4) 0.74714(17) 0.0088(7) Uani 1 1 d .
O5 O 1.6009(4) 0.3625(5) 0.60350(18) 0.0148(8) Uani 1 1 d .
O4 O 1.5187(4) 0.4359(5) 0.81758(18) 0.0170(9) Uani 1 1 d .
O3A O 1.3820(7) 0.2438(9) 0.8597(3) 0.041(2) Uani 0.775(12) 1 d P
O3B O 1.730(2) 0.489(3) 0.8757(10) 0.030(6) Uani 0.225(12) 1 d P
O2 O 1.6270(6) 0.2203(7) 0.8749(2) 0.0438(15) Uani 1 1 d .
O1 O 1.5186(6) 0.4224(6) 0.9269(2) 0.0307(11) Uani 1 1 d .
O21 O 1.5030(3) -0.0590(4) 0.76216(16) 0.0072(7) Uani 1 1 d .
O20 O 1.4794(4) -0.0040(4) 0.65103(18) 0.0128(8) Uani 1 1 d .
O19 O 1.9365(4) 0.3101(5) 0.55304(18) 0.0168(8) Uani 1 1 d .
O18 O 1.8520(3) 0.3259(5) 0.64991(17) 0.0097(7) Uani 1 1 d .
O17 O 1.4552(5) 0.6852(5) 0.6244(2) 0.0240(10) Uani 1 1 d .
O16 O 1.0915(4) 0.3371(4) 0.64745(17) 0.0088(7) Uani 1 1 d .
O15 O 1.6651(4) 0.3119(7) 0.5004(2) 0.0304(12) Uani 1 1 d .
O14 O 1.4353(4) 0.3357(7) 0.5128(2) 0.0290(11) Uani 1 1 d .
O13 O 1.1932(4) 0.3342(7) 0.5063(2) 0.0319(12) Uani 1 1 d .
B1 B 1.2342(6) 0.6244(7) 0.7538(3) 0.0077(11) Uani 1 1 d .
B2 B 1.4910(6) 0.0700(6) 0.7112(3) 0.0071(11) Uani 1 1 d .
B8 B 1.7668(6) 0.6253(7) 0.7507(3) 0.0076(11) Uani 1 1 d .
B7 B 1.8619(6) 0.3616(7) 0.7169(3) 0.0084(11) Uani 1 1 d .
B6 B 1.1200(6) 0.3625(7) 0.7154(3) 0.0081(11) Uani 1 1 d .
B5 B 1.9628(6) 0.3223(7) 0.6168(3) 0.0089(11) Uani 1 1 d .
B4 B 1.3180(7) 0.3482(10) 0.5407(3) 0.0209(15) Uani 1 1 d .
B3 B 1.5704(7) 0.3365(9) 0.5401(3) 0.0185(14) Uani 1 1 d .
O1W O 1.2781(14) 0.0296(18) 0.5505(6) 0.060(3) Uiso 0.50 1 d P
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'
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'
La La -0.2871 2.4523 '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
O17 La1 O4 136.86(14) . .
O17 La1 O9 70.43(15) . .
O4 La1 O9 140.12(13) . .
O17 La1 O12 94.65(14) . .
O4 La1 O12 77.93(12) . .
O9 La1 O12 70.11(12) . .
O17 La1 O11 99.38(14) . .
O4 La1 O11 77.75(12) . .
O9 La1 O11 134.17(12) . .
O12 La1 O11 155.08(11) . .
O17 La1 O5 75.24(15) . .
O4 La1 O5 138.47(13) . .
O9 La1 O5 64.21(13) . .
O12 La1 O5 134.03(12) . .
O11 La1 O5 69.97(12) . .
O17 La1 O8 142.82(14) . .
O4 La1 O8 74.87(12) . .
O9 La1 O8 96.80(13) . .
O12 La1 O8 114.15(11) . .
O11 La1 O8 63.97(11) . .
O5 La1 O8 67.89(12) . .
O17 La1 O10 138.18(14) . .
O4 La1 O10 76.61(12) . .
O9 La1 O10 68.46(12) . .
O12 La1 O10 64.35(11) . .
O11 La1 O10 114.56(11) . .
O5 La1 O10 93.50(12) . .
O8 La1 O10 51.52(11) . .
O17 La1 O6 72.86(14) . .
O4 La1 O6 72.55(12) . .
O9 La1 O6 143.23(12) . .
O12 La1 O6 115.53(11) . .
O11 La1 O6 50.97(11) . .
O5 La1 O6 104.21(12) . .
O8 La1 O6 111.29(12) . .
O10 La1 O6 148.14(11) . .
O17 La1 O7 71.78(14) . .
O4 La1 O7 70.73(12) . .
O9 La1 O7 104.61(12) . .
O12 La1 O7 51.24(11) . .
O11 La1 O7 114.47(11) . .
O5 La1 O7 147.01(12) . .
O8 La1 O7 144.78(11) . .
O10 La1 O7 111.69(12) . .
O6 La1 O7 65.11(11) . .
O17 La1 B8 87.07(16) . .
O4 La1 B8 72.18(14) . .
O9 La1 B8 147.36(14) . .
O12 La1 B8 137.16(14) . .
O11 La1 B8 25.36(13) . .
O5 La1 B8 87.81(14) . .
O8 La1 B8 86.95(14) . .
O10 La1 B8 133.39(13) . .
O6 La1 B8 25.68(13) . .
O7 La1 B8 89.62(14) . .
O17 La1 B1 83.66(16) . .
O4 La1 B1 71.53(14) . .
O9 La1 B1 87.93(14) . .
O12 La1 B1 25.53(13) . .
O11 La1 B1 136.59(14) . .
O5 La1 B1 149.27(13) . .
O8 La1 B1 131.91(13) . .
O10 La1 B1 87.47(14) . .
O6 La1 B1 90.25(14) . .
O7 La1 B1 25.76(13) . .
B8 La1 B1 113.48(15) . .
Cl1B Cl1A O1 76.2(4) . .
Cl1B Cl1A O3A 170.9(5) . .
O1 Cl1A O3A 112.6(4) . .
Cl1B Cl1A O4 69.5(3) . .
O1 Cl1A O4 110.1(3) . .
O3A Cl1A O4 108.0(3) . .
Cl1B Cl1A O2 61.9(4) . .
O1 Cl1A O2 108.0(3) . .
O3A Cl1A O2 111.7(4) . .
O4 Cl1A O2 106.2(3) . .
Cl1A Cl1B O2 72.8(5) . .
Cl1A Cl1B O3B 167.5(11) . .
O2 Cl1B O3B 119.6(10) . .
Cl1A Cl1B O4 66.5(3) . .
O2 Cl1B O4 110.6(5) . .
O3B Cl1B O4 105.3(9) . .
Cl1A Cl1B O1 60.9(4) . .
O2 Cl1B O1 105.4(5) . .
O3B Cl1B O1 113.8(10) . .
O4 Cl1B O1 100.5(4) . .
B1 O12 B6 125.0(4) . .
B1 O12 La1 100.7(3) . .
B6 O12 La1 134.3(3) . .
B8 O11 B7 124.7(4) . .
B8 O11 La1 100.3(3) . .
B7 O11 La1 135.0(3) . .
B1 O10 B2 122.2(4) 2_746 .
B1 O10 La1 135.5(3) 2_746 .
B2 O10 La1 99.5(3) . .
B4 O9 La1 141.0(4) . .
B8 O8 B2 121.0(4) 2_846 .
B8 O8 La1 137.2(3) 2_846 .
B2 O8 La1 100.3(3) . .
B1 O7 B6 122.0(4) . 2_756
B1 O7 La1 95.2(3) . .
B6 O7 La1 141.0(3) 2_756 .
B8 O6 B7 121.6(4) . 2_856
B8 O6 La1 95.1(3) . .
B7 O6 La1 139.2(3) 2_856 .
B3 O5 La1 140.4(4) . .
Cl1A O4 Cl1B 44.0(3) . .
Cl1A O4 La1 146.7(2) . .
Cl1B O4 La1 146.7(4) . .
Cl1B O2 Cl1A 45.3(3) . .
Cl1A O1 Cl1B 43.0(3) . .
B7 O21 B6 115.9(4) 2_846 2_746
B7 O21 B2 120.5(4) 2_846 .
B6 O21 B2 122.4(4) 2_746 .
B5 O18 B7 123.5(4) . .
B5 O16 B6 123.2(4) 1_455 .
B4 O14 B3 129.3(5) . .
O10 B1 O7 125.3(5) 2_756 .
O10 B1 O12 122.0(5) 2_756 .
O7 B1 O12 112.7(4) . .
O10 B1 La1 173.0(4) 2_756 .
O7 B1 La1 59.0(3) . .
O12 B1 La1 53.8(2) . .
O20 B2 O8 112.4(4) . .
O20 B2 O10 112.4(4) . .
O8 B2 O10 103.5(4) . .
O20 B2 O21 110.0(4) . .
O8 B2 O21 109.1(4) . .
O10 B2 O21 109.2(4) . .
O8 B8 O6 124.5(5) 2_856 .
O8 B8 O11 122.1(5) 2_856 .
O6 B8 O11 113.4(4) . .
O8 B8 La1 173.0(4) 2_856 .
O6 B8 La1 59.3(3) . .
O11 B8 La1 54.3(2) . .
O18 B7 O6 110.4(4) . 2_846
O18 B7 O11 107.0(4) . .
O6 B7 O11 111.2(4) 2_846 .
O18 B7 O21 109.4(4) . 2_856
O6 B7 O21 108.9(4) 2_846 2_856
O11 B7 O21 110.0(4) . 2_856
O7 B6 O16 111.1(4) 2_746 .
O7 B6 O12 111.6(4) 2_746 .
O16 B6 O12 107.7(4) . .
O7 B6 O21 108.8(4) 2_746 2_756
O16 B6 O21 108.3(4) . 2_756
O12 B6 O21 109.3(4) . 2_756
O16 B5 O19 122.8(5) 1_655 .
O16 B5 O18 120.1(5) 1_655 .
O19 B5 O18 117.0(5) . .
O13 B4 O9 117.6(5) . .
O13 B4 O14 120.9(6) . .
O9 B4 O14 121.6(5) . .
O15 B3 O5 124.1(5) . .
O15 B3 O14 115.8(5) . .
O5 B3 O14 120.1(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
La1 O17 2.429(4) .
La1 O4 2.510(4) .
La1 O9 2.573(4) .
La1 O12 2.587(4) .
La1 O11 2.591(4) .
La1 O5 2.613(4) .
La1 O8 2.658(4) .
La1 O10 2.675(4) .
La1 O6 2.707(4) .
La1 O7 2.712(4) .
La1 B8 3.138(6) .
La1 B1 3.150(6) .
Cl1A Cl1B 1.100(6) .
Cl1A O1 1.409(5) .
Cl1A O3A 1.429(7) .
Cl1A O4 1.451(4) .
Cl1A O2 1.477(6) .
Cl1B O2 1.364(8) .
Cl1B O3B 1.46(2) .
Cl1B O4 1.482(7) .
Cl1B O1 1.567(8) .
O12 B1 1.382(7) .
O12 B6 1.466(7) .
O11 B8 1.366(7) .
O11 B7 1.466(6) .
O10 B1 1.344(7) 2_746
O10 B2 1.476(6) .
O9 B4 1.365(8) .
O8 B8 1.362(7) 2_846
O8 B2 1.475(6) .
O7 B1 1.375(7) .
O7 B6 1.453(7) 2_756
O6 B8 1.365(7) .
O6 B7 1.462(7) 2_856
O5 B3 1.371(8) .
O21 B7 1.503(6) 2_846
O21 B6 1.504(6) 2_746
O21 B2 1.518(6) .
O20 B2 1.419(7) .
O19 B5 1.362(7) .
O18 B5 1.373(7) .
O18 B7 1.457(7) .
O16 B5 1.361(7) 1_455
O16 B6 1.463(7) .
O15 B3 1.352(8) .
O14 B4 1.369(8) .
O14 B3 1.387(7) .
O13 B4 1.360(8) .
B1 O10 1.344(7) 2_756
B8 O8 1.362(7) 2_856
B7 O6 1.462(7) 2_846
B7 O21 1.503(6) 2_856
B6 O7 1.453(7) 2_746
B6 O21 1.504(6) 2_756
B5 O16 1.361(7) 1_655
