#------------------------------------------------------------------------------
#$Date: 2016-02-16 21:30:59 +0100 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://saulius.grazulis.lt/cod-secondary/cif/4/31/57/4315700.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_4315700
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 O2 Tm'
_chemical_formula_weight         238.40
_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                   12.5628(11)
_cell_length_b                   3.5645(3)
_cell_length_c                   6.2015(5)
_cell_measurement_temperature    140(1)
_cell_volume                     277.70(4)
_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 0.997
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Bruker D8 with APEXII CCD'
_diffrn_measurement_method       '\w 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  0.0221
_diffrn_reflns_av_sigmaI/netI    0.0129
_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            2723
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.62
_diffrn_reflns_theta_min         3.24
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    32.616
_exptl_absorpt_correction_T_max  0.2450
_exptl_absorpt_correction_T_min  0.1113
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.03 (Sheldrick, 2001)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    5.702
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             416
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.115
_refine_diff_density_min         -2.403
_refine_diff_density_rms         0.339
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     29
_refine_ls_number_reflns         401
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.0203
_refine_ls_R_factor_gt           0.0170
_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/[\s^2^(Fo^2^)+(0.0299P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0447
_refine_ls_wR_factor_ref         0.0466
_reflns_number_gt                338
_reflns_number_total             401
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901617c_si_007_11.cif
_cod_data_source_block           apx064a
_cod_original_formula_sum        'H2 Cl O2 Tm'
_cod_database_code               4315700
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
Tm1 Tm 0.054192(18) 0.7500 0.24995(3) 0.00293(13) Uani 1 2 d S . .
Cl1 Cl 0.21295(10) 1.2500 0.39105(18) 0.0056(2) Uani 1 2 d S . .
O1 O 0.0801(3) 0.2500 0.0025(5) 0.0046(7) Uani 1 2 d S . .
O2 O -0.0464(2) 0.2500 0.3691(6) 0.0042(8) Uani 1 2 d S . .
H1 H 0.138(7) 0.2500 -0.037(14) 0.060 Uiso 1 2 d S . .
H2 H -0.111(7) 0.2500 0.334(17) 0.060 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
Tm1 0.00346(18) 0.00346(19) 0.00187(18) 0.000 -0.00045(7) 0.000
Cl1 0.0048(5) 0.0068(5) 0.0051(5) 0.000 -0.0009(5) 0.000
O1 0.0028(16) 0.0069(18) 0.0042(16) 0.000 0.0014(14) 0.000
O2 0.0050(17) 0.005(2) 0.0023(18) 0.000 -0.0005(12) 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'
Tm Tm -0.3139 5.2483 '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
O1 Tm1 O2 79.42(10) 5_565 . ?
O1 Tm1 O2 79.42(10) 5_565 1_565 ?
O2 Tm1 O2 101.23(13) . 1_565 ?
O1 Tm1 O2 130.47(10) 5_565 5_566 ?
O2 Tm1 O2 69.95(11) . 5_566 ?
O2 Tm1 O2 69.95(11) 1_565 5_566 ?
O1 Tm1 O1 70.19(11) 5_565 1_565 ?
O2 Tm1 O1 149.59(11) . 1_565 ?
O2 Tm1 O1 72.67(10) 1_565 1_565 ?
O2 Tm1 O1 130.65(6) 5_566 1_565 ?
O1 Tm1 O1 70.19(11) 5_565 . ?
O2 Tm1 O1 72.67(10) . . ?
O2 Tm1 O1 149.59(11) 1_565 . ?
O2 Tm1 O1 130.65(6) 5_566 . ?
O1 Tm1 O1 97.30(12) 1_565 . ?
O1 Tm1 Cl1 136.97(3) 5_565 1_545 ?
O2 Tm1 Cl1 78.41(7) . 1_545 ?
O2 Tm1 Cl1 141.08(9) 1_565 1_545 ?
O2 Tm1 Cl1 73.67(6) 5_566 1_545 ?
O1 Tm1 Cl1 125.38(8) 1_565 1_545 ?
O1 Tm1 Cl1 68.17(8) . 1_545 ?
O1 Tm1 Cl1 136.97(4) 5_565 . ?
O2 Tm1 Cl1 141.08(9) . . ?
O2 Tm1 Cl1 78.41(7) 1_565 . ?
O2 Tm1 Cl1 73.67(6) 5_566 . ?
O1 Tm1 Cl1 68.18(8) 1_565 . ?
O1 Tm1 Cl1 125.38(8) . . ?
Cl1 Tm1 Cl1 78.59(3) 1_545 . ?
O1 Tm1 Tm1 90.0 5_565 1_545 ?
O2 Tm1 Tm1 39.39(6) . 1_545 ?
O2 Tm1 Tm1 140.61(6) 1_565 1_545 ?
O2 Tm1 Tm1 90.0 5_566 1_545 ?
O1 Tm1 Tm1 138.65(6) 1_565 1_545 ?
O1 Tm1 Tm1 41.35(6) . 1_545 ?
Cl1 Tm1 Tm1 50.705(16) 1_545 1_545 ?
Cl1 Tm1 Tm1 129.294(16) . 1_545 ?
O1 Tm1 Tm1 90.0 5_565 1_565 ?
O2 Tm1 Tm1 140.61(6) . 1_565 ?
O2 Tm1 Tm1 39.39(6) 1_565 1_565 ?
O2 Tm1 Tm1 90.0 5_566 1_565 ?
O1 Tm1 Tm1 41.35(6) 1_565 1_565 ?
O1 Tm1 Tm1 138.65(6) . 1_565 ?
Cl1 Tm1 Tm1 129.295(16) 1_545 1_565 ?
Cl1 Tm1 Tm1 50.705(16) . 1_565 ?
Tm1 Tm1 Tm1 180.0 1_545 1_565 ?
O1 Tm1 Tm1 35.71(5) 5_565 5_565 ?
O2 Tm1 Tm1 72.82(9) . 5_565 ?
O2 Tm1 Tm1 115.13(9) 1_565 5_565 ?
O2 Tm1 Tm1 142.62(5) 5_566 5_565 ?
O1 Tm1 Tm1 82.81(7) 1_565 5_565 ?
O1 Tm1 Tm1 34.48(8) . 5_565 ?
Cl1 Tm1 Tm1 102.071(19) 1_545 5_565 ?
Cl1 Tm1 Tm1 143.04(2) . 5_565 ?
Tm1 Tm1 Tm1 62.240(4) 1_545 5_565 ?
Tm1 Tm1 Tm1 117.760(4) 1_565 5_565 ?
O1 Tm1 Tm1 35.71(5) 5_565 5_575 ?
O2 Tm1 Tm1 115.13(9) . 5_575 ?
O2 Tm1 Tm1 72.82(9) 1_565 5_575 ?
O2 Tm1 Tm1 142.62(5) 5_566 5_575 ?
O1 Tm1 Tm1 34.47(8) 1_565 5_575 ?
O1 Tm1 Tm1 82.81(7) . 5_575 ?
Cl1 Tm1 Tm1 143.04(2) 1_545 5_575 ?
Cl1 Tm1 Tm1 102.072(19) . 5_575 ?
Tm1 Tm1 Tm1 117.760(3) 1_545 5_575 ?
Tm1 Tm1 Tm1 62.240(3) 1_565 5_575 ?
Tm1 Tm1 Tm1 55.521(7) 5_565 5_575 ?
Tm1 Cl1 Tm1 78.59(3) 1_565 . ?
Tm1 O1 Tm1 109.81(11) 5_565 1_545 ?
Tm1 O1 Tm1 109.81(11) 5_565 . ?
Tm1 O1 Tm1 97.30(12) 1_545 . ?
Tm1 O2 Tm1 101.23(13) . 1_545 ?
Tm1 O2 Tm1 110.05(11) . 5_566 ?
Tm1 O2 Tm1 110.05(11) 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
Tm1 O1 2.302(4) 5_565 ?
Tm1 O2 2.306(2) . ?
Tm1 O2 2.306(2) 1_565 ?
Tm1 O2 2.365(4) 5_566 ?
Tm1 O1 2.374(2) 1_565 ?
Tm1 O1 2.374(2) . ?
Tm1 Cl1 2.8142(9) 1_545 ?
Tm1 Cl1 2.8142(9) . ?
Tm1 Tm1 3.5645(3) 1_545 ?
Tm1 Tm1 3.5645(3) 1_565 ?
Tm1 Tm1 3.8264(4) 5_565 ?
Tm1 Tm1 3.8264(4) 5_575 ?
Cl1 Tm1 2.8142(9) 1_565 ?
O1 Tm1 2.302(4) 5_565 ?
O1 Tm1 2.374(2) 1_545 ?
O2 Tm1 2.306(2) 1_545 ?
O2 Tm1 2.365(4) 5_566 ?
