#------------------------------------------------------------------------------
#$Date: 2016-02-16 21:30:59 +0100 (mar 16 de feb de 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/57/4315702.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_4315702
loop_
_publ_author_name
'Ralph A. Zehnder'
'David L. Clark'
'Brian L. Scott'
'Robert J. Donohoe'
'Phillip D. Palmer'
'Wolfgang H. Runde'
'David E. Hobart'
_publ_section_title
;
 Investigation of the Structural Properties of an Extended Series of
 Lanthanide Bis-hydroxychlorides Ln(OH)2Cl (Ln = Nd-Lu, except Pm and Sm)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4781
_journal_page_last               4790
_journal_paper_doi               10.1021/ic901617c
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'Cl H2 Lu O2'
_chemical_formula_weight         244.44
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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            4
_cell_length_a                   12.609(3)
_cell_length_b                   3.5093(8)
_cell_length_c                   6.1839(14)
_cell_measurement_temperature    140(1)
_cell_volume                     273.63(11)
_computing_cell_refinement       'SAINT+, v. 7.06 (Bruker AXS, 2001)'
_computing_data_collection       'APEX II, v. 1.08 (Bruker AXS, 2003)'
_computing_data_reduction        'SAINT+, v. 7.06 (Bruker AXS, 2001)'
_computing_molecular_graphics    'SHELXTL, v. 6.10, (Bruker AXS, 2000)'
_computing_publication_material  'SHELXTL, v. 6.10, (Bruker AXS, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      140(1)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Bruker D8 with APEXII CCD'
_diffrn_measurement_method       'ω scans'
_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  0.0321
_diffrn_reflns_av_sigmaI/netI    0.0233
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            2435
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.53
_diffrn_reflns_theta_min         3.23
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    36.755
_exptl_absorpt_correction_T_max  0.4052
_exptl_absorpt_correction_T_min  0.0670
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.03 (Sheldrick, 2001)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    5.933
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             424
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         3.823
_refine_diff_density_min         -2.044
_refine_diff_density_rms         0.482
_refine_ls_extinction_coef       0.0055(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.175
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     30
_refine_ls_number_reflns         393
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.166
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0259
_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)+(0.0485P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0754
_refine_ls_wR_factor_ref         0.0782
_reflns_number_gt                320
_reflns_number_total             393
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901617c_si_007_13.cif
_cod_data_source_block           apx142a
_cod_original_cell_volume        273.64(11)
_cod_original_formula_sum        'H2 Cl Lu O2'
_cod_database_code               4315702
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
Lu1 Lu 0.05320(3) 0.7500 0.24981(5) 0.0036(3) Uani 1 2 d S . .
Cl1 Cl 0.21140(15) 1.2500 0.3866(3) 0.0058(5) Uani 1 2 d S . .
O1 O 0.0799(4) 0.2500 0.0008(9) 0.0049(11) Uani 1 2 d SU . .
O2 O -0.0464(4) 0.2500 0.3702(11) 0.0080(14) Uani 1 2 d S . .
H1 H 0.143(16) 0.2500 -0.04(3) 0.100 Uiso 1 2 d S . .
H2 H -0.116(17) 0.2500 0.33(3) 0.100 Uiso 1 2 d S . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Lu1 0.0054(3) 0.0044(4) 0.0011(3) 0.000 -0.00015(11) 0.000
Cl1 0.0084(8) 0.0043(10) 0.0049(8) 0.000 -0.0007(9) 0.000
O1 0.006(2) 0.007(3) 0.001(2) 0.000 0.002(2) 0.000
O2 0.009(3) 0.013(4) 0.002(3) 0.000 0.000(2) 0.000
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 '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 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Lu Lu -0.4720 5.8584 '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
O2 Lu1 O2 100.5(2) . 1_565 ?
O2 Lu1 O1 79.45(17) . 5_565 ?
O2 Lu1 O1 79.45(17) 1_565 5_565 ?
O2 Lu1 O2 69.76(19) . 5_566 ?
O2 Lu1 O2 69.76(19) 1_565 5_566 ?
O1 Lu1 O2 130.63(18) 5_565 5_566 ?
O2 Lu1 O1 73.72(17) . . ?
O2 Lu1 O1 149.70(19) 1_565 . ?
O1 Lu1 O1 70.26(16) 5_565 . ?
O2 Lu1 O1 131.11(11) 5_566 . ?
O2 Lu1 O1 149.70(19) . 1_565 ?
O2 Lu1 O1 73.72(17) 1_565 1_565 ?
O1 Lu1 O1 70.26(16) 5_565 1_565 ?
O2 Lu1 O1 131.11(11) 5_566 1_565 ?
O1 Lu1 O1 96.1(2) . 1_565 ?
O2 Lu1 Cl1 79.11(12) . 1_545 ?
O2 Lu1 Cl1 141.13(16) 1_565 1_545 ?
O1 Lu1 Cl1 137.01(6) 5_565 1_545 ?
O2 Lu1 Cl1 73.91(10) 5_566 1_545 ?
O1 Lu1 Cl1 68.13(13) . 1_545 ?
O1 Lu1 Cl1 124.33(12) 1_565 1_545 ?
O2 Lu1 Cl1 141.13(16) . . ?
O2 Lu1 Cl1 79.11(12) 1_565 . ?
O1 Lu1 Cl1 137.01(6) 5_565 . ?
O2 Lu1 Cl1 73.92(10) 5_566 . ?
O1 Lu1 Cl1 124.33(12) . . ?
O1 Lu1 Cl1 68.13(13) 1_565 . ?
Cl1 Lu1 Cl1 78.01(5) 1_545 . ?
O2 Lu1 Lu1 39.77(10) . 1_545 ?
O2 Lu1 Lu1 140.24(10) 1_565 1_545 ?
O1 Lu1 Lu1 90.0 5_565 1_545 ?
O2 Lu1 Lu1 90.0 5_566 1_545 ?
O1 Lu1 Lu1 41.93(10) . 1_545 ?
O1 Lu1 Lu1 138.07(10) 1_565 1_545 ?
Cl1 Lu1 Lu1 51.00(3) 1_545 1_545 ?
Cl1 Lu1 Lu1 129.00(3) . 1_545 ?
O2 Lu1 Lu1 140.24(10) . 1_565 ?
O2 Lu1 Lu1 39.77(10) 1_565 1_565 ?
O1 Lu1 Lu1 90.0 5_565 1_565 ?
O2 Lu1 Lu1 90.0 5_566 1_565 ?
O1 Lu1 Lu1 138.07(10) . 1_565 ?
O1 Lu1 Lu1 41.93(10) 1_565 1_565 ?
Cl1 Lu1 Lu1 129.00(3) 1_545 1_565 ?
Cl1 Lu1 Lu1 51.00(3) . 1_565 ?
Lu1 Lu1 Lu1 180.0 1_545 1_565 ?
Lu1 Cl1 Lu1 78.01(5) 1_565 . ?
Lu1 O1 Lu1 109.74(16) 5_565 . ?
Lu1 O1 Lu1 109.74(16) 5_565 1_545 ?
Lu1 O1 Lu1 96.1(2) . 1_545 ?
Lu1 O2 Lu1 100.5(2) . 1_545 ?
Lu1 O2 Lu1 110.24(19) . 5_566 ?
Lu1 O2 Lu1 110.24(19) 1_545 5_566 ?
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
Lu1 O2 2.283(3) . ?
Lu1 O2 2.283(3) 1_565 ?
Lu1 O1 2.285(6) 5_565 ?
Lu1 O2 2.351(7) 5_566 ?
Lu1 O1 2.359(4) . ?
Lu1 O1 2.359(4) 1_565 ?
Lu1 Cl1 2.7880(16) 1_545 ?
Lu1 Cl1 2.7880(16) . ?
Lu1 Lu1 3.5093(8) 1_545 ?
Lu1 Lu1 3.5093(8) 1_565 ?
Cl1 Lu1 2.7879(16) 1_565 ?
O1 Lu1 2.285(6) 5_565 ?
O1 Lu1 2.359(4) 1_545 ?
O2 Lu1 2.283(3) 1_545 ?
O2 Lu1 2.351(7) 5_566 ?
