#------------------------------------------------------------------------------
#$Date: 2024-11-29 04:51:50 +0200 (Fri, 29 Nov 2024) $
#$Revision: 296161 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/33/1573328.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_1573328
_journal_paper_doi               10.1107/S2056989024011319
_chemical_formula_iupac          '[La Cl (H2 O)7] Cl2'
_chemical_formula_moiety         'La Cl H14 O7 2+, 2(Cl -)'
_chemical_formula_sum            'Cl3 H14 La O7'
_chemical_formula_weight         371.37
_chemical_name_systematic
;
Di-μ-chlorido-bis[heptaaqualanthanum(III)] tetrachloride
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_cell_angle_alpha                70.507(2)
_cell_angle_beta                 73.098(2)
_cell_angle_gamma                81.522(2)
_cell_formula_units_Z            2
_cell_length_a                   7.9432(5)
_cell_length_b                   8.2316(4)
_cell_length_c                   9.2203(5)
_cell_measurement_reflns_used    9869
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      23.647
_cell_measurement_theta_min      2.351
_cell_volume                     542.92(5)
_computing_cell_refinement
;
SAINT V8.40B (Bruker, 2016)
;
_computing_data_reduction
;
SAINT V8.40B (Bruker, 2016)
;
_computing_molecular_graphics
;
CrystalMaker (Palmer, 2014)
;
_computing_publication_material
;
PublCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL 2018/1 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT 2018/2 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Venture Duo'
_diffrn_measurement_method       ω
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56086
_diffrn_reflns_av_R_equivalents  0.0691
_diffrn_reflns_av_unetI/netI     0.0257
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            43724
_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         23.712
_diffrn_reflns_theta_min         2.118
_diffrn_source_current           0.91
_diffrn_source_power             0.0455
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    2.424
_exptl_absorpt_correction_T_max  0.0636
_exptl_absorpt_correction_T_min  0.0439
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker, 2016)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.272
_exptl_crystal_description       plate
_exptl_crystal_F_000             356
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.397
_refine_diff_density_min         -0.442
_refine_ls_extinction_coef       0.0070(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method
;
SHELXL-2018/1 (Sheldrick 2015b)
;
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     157
_refine_ls_number_reflns         3350
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0196
_refine_ls_R_factor_gt           0.0159
_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)+(0.0128P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0314
_refine_ls_wR_factor_ref         0.0323
_reflns_number_gt                3078
_reflns_number_total             3350
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            hb8106.cif
_cod_data_source_block           La
_cod_original_formula_sum        'La Cl3 H14 O7'
_cod_database_code               1573328
_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   0.292
_shelx_estimated_absorpt_t_max   0.868
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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
La La1 0.21799(2) 0.18615(2) 0.32361(2) 0.00928(4) Uani d 1 . .
Cl Cl1 -0.14698(6) 0.17974(5) 0.51434(5) 0.01189(8) Uani d 1 . .
Cl Cl2 0.21093(6) 0.77753(5) 0.03491(5) 0.01465(8) Uani d 1 . .
Cl Cl3 0.34270(6) 0.38778(5) 0.71161(5) 0.01506(9) Uani d 1 . .
O O1 0.0304(2) 0.42402(17) 0.17472(17) 0.0149(3) Uani d 1 . .
O O2 0.07092(19) 0.08113(17) 0.16194(16) 0.0148(3) Uani d 1 . .
O O3 0.2234(2) 0.46276(18) 0.38494(18) 0.0188(3) Uani d 1 . .
O O4 0.2311(2) 0.09299(18) 0.61748(16) 0.0153(3) Uani d 1 . .
O O5 0.3868(2) 0.35162(17) 0.04773(16) 0.0145(3) Uani d 1 . .
O O6 0.5212(2) 0.2280(2) 0.34138(17) 0.0173(3) Uani d 1 . .
O O7 0.4532(2) -0.01065(18) 0.19716(17) 0.0164(3) Uani d 1 . .
H H1A -0.060(4) 0.447(3) 0.219(3) 0.030(7) Uiso d 1 . .
H H1B 0.077(4) 0.509(3) 0.119(3) 0.028(7) Uiso d 1 . .
H H2A 0.015(4) 0.143(3) 0.103(3) 0.033(7) Uiso d 1 . .
H H2B 0.116(4) 0.003(4) 0.131(3) 0.035(7) Uiso d 1 . .
H H3A 0.259(4) 0.470(4) 0.458(3) 0.042(8) Uiso d 1 . .
H H3B 0.199(4) 0.553(4) 0.330(4) 0.051(9) Uiso d 1 . .
H H4A 0.144(4) 0.052(3) 0.677(3) 0.027(7) Uiso d 1 . .
H H4B 0.261(4) 0.171(3) 0.644(3) 0.030(7) Uiso d 1 . .
H H5A 0.360(4) 0.367(4) -0.033(3) 0.038(8) Uiso d 1 . .
H H5B 0.485(4) 0.339(4) 0.031(4) 0.046(9) Uiso d 1 . .
H H6A 0.549(5) 0.312(4) 0.344(4) 0.059(11) Uiso d 1 . .
H H6B 0.596(4) 0.151(4) 0.352(3) 0.048(9) Uiso d 1 . .
H H7A 0.535(4) 0.031(4) 0.131(3) 0.036(8) Uiso d 1 . .
H H7B 0.464(5) -0.115(4) 0.228(4) 0.057(10) Uiso d 1 . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cl Cl 0.1009 0.0992 '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'
La La -0.5913 1.6253 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0058 0.0036 '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 La1 Cl1 . 2_556 73.941(12) ?
O1 La1 Cl1 . 2_556 128.72(4) ?
O1 La1 Cl1 . . 69.96(4) ?
O1 La1 O2 . . 67.52(4) ?
O1 La1 O4 . . 130.45(4) ?
O1 La1 O7 . . 124.76(4) ?
O2 La1 Cl1 . . 79.41(3) ?
O2 La1 Cl1 . 2_556 71.07(3) ?
O2 La1 O4 . . 135.97(5) ?
O2 La1 O7 . . 74.71(4) ?
O3 La1 Cl1 . 2_556 140.68(4) ?
O3 La1 Cl1 . . 84.97(4) ?
O3 La1 O1 . . 70.08(5) ?
O3 La1 O2 . . 137.58(4) ?
O3 La1 O4 . . 74.18(5) ?
O3 La1 O6 . . 68.30(5) ?
O3 La1 O7 . . 134.49(5) ?
O4 La1 Cl1 . 2_556 68.28(3) ?
O4 La1 Cl1 . . 73.83(4) ?
O5 La1 Cl1 . . 136.61(3) ?
O5 La1 Cl1 . 2_556 133.83(3) ?
O5 La1 O1 . . 66.80(5) ?
O5 La1 O2 . . 81.23(5) ?
O5 La1 O3 . . 83.78(5) ?
O5 La1 O4 . . 140.90(5) ?
O5 La1 O6 . . 72.77(5) ?
O5 La1 O7 . . 68.91(5) ?
O6 La1 Cl1 . . 138.86(3) ?
O6 La1 Cl1 . 2_556 107.32(4) ?
O6 La1 O1 . . 123.86(5) ?
O6 La1 O2 . . 141.04(4) ?
O6 La1 O4 . . 69.20(5) ?
O6 La1 O7 . . 69.14(5) ?
O7 La1 Cl1 . 2_556 68.54(4) ?
O7 La1 Cl1 . . 139.55(4) ?
O7 La1 O4 . . 104.74(4) ?
La1 Cl1 La1 . 2_556 106.059(12) ?
La1 O1 H1A . . 119(2) ?
La1 O1 H1B . . 117(2) ?
H1A O1 H1B . . 109(3) ?
La1 O2 H2A . . 124.0(19) ?
La1 O2 H2B . . 119(2) ?
H2A O2 H2B . . 110(2) ?
La1 O3 H3A . . 125.3(19) ?
La1 O3 H3B . . 123(2) ?
H3A O3 H3B . . 112(3) ?
La1 O4 H4A . . 112.1(19) ?
La1 O4 H4B . . 114.3(17) ?
H4A O4 H4B . . 112(2) ?
La1 O5 H5A . . 126(2) ?
La1 O5 H5B . . 116(2) ?
H5A O5 H5B . . 108(3) ?
La1 O6 H6A . . 124(3) ?
La1 O6 H6B . . 123(2) ?
H6A O6 H6B . . 112(3) ?
La1 O7 H7A . . 119(2) ?
La1 O7 H7B . . 128(2) ?
H7A O7 H7B . . 113(3) ?
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
La1 Cl1 2_556 2.9376(4) ?
La1 Cl1 . 2.9187(5) y
La1 O1 . 2.5443(13) y
La1 O2 . 2.5504(13) y
La1 O3 . 2.5315(13) y
La1 O4 . 2.5873(13) y
La1 O5 . 2.5233(14) y
La1 O6 . 2.5413(15) y
La1 O7 . 2.5643(13) y
O1 H1A . 0.75(3) ?
O1 H1B . 0.79(3) ?
O2 H2A . 0.80(3) ?
O2 H2B . 0.79(3) ?
O3 H3A . 0.82(3) ?
O3 H3B . 0.78(3) ?
O4 H4A . 0.78(3) ?
O4 H4B . 0.84(3) ?
O5 H5A . 0.80(3) ?
O5 H5B . 0.75(3) ?
O6 H6A . 0.77(3) ?
O6 H6B . 0.80(3) ?
O7 H7A . 0.78(3) ?
O7 H7B . 0.81(3) ?
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
_geom_hbond_publ_flag
O1 H1A Cl3 2_566 0.75(3) 2.48(3) 3.1947(15) 161(3) yes
O1 H1B Cl2 . 0.79(3) 2.38(3) 3.1365(16) 161(2) yes
O2 H2A Cl2 2_565 0.80(3) 2.38(3) 3.1378(14) 157(3) yes
O2 H2B Cl2 1_545 0.79(3) 2.26(3) 3.0382(13) 172(3) yes
O3 H3A Cl3 . 0.82(3) 2.47(3) 3.2552(15) 160(3) yes
O3 H3B Cl1 2_566 0.78(3) 2.92(3) 3.2954(13) 112(2) yes
O3 H3B Cl2 . 0.78(3) 2.72(3) 3.4160(16) 150(3) yes
O4 H4A O2 2_556 0.78(3) 2.08(3) 2.859(2) 174(3) yes
O4 H4B Cl3 . 0.84(3) 2.31(3) 3.1488(15) 179(2) yes
O5 H5A Cl3 1_554 0.80(3) 2.34(3) 3.1308(14) 167(3) yes
O5 H5B Cl2 2_665 0.75(3) 2.44(3) 3.1690(15) 163(3) yes
O5 H5B O5 2_665 0.75(3) 2.67(3) 2.986(3) 108(2) yes
O6 H6A Cl3 2_666 0.77(3) 2.57(3) 3.3288(16) 168(3) yes
O6 H6B Cl1 1_655 0.80(3) 2.93(3) 3.3705(14) 117(2) yes
O6 H6B O4 2_656 0.80(3) 2.24(3) 3.038(2) 169(3) yes
