#------------------------------------------------------------------------------
#$Date: 2016-02-16 21:30:59 +0100 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://saulius.grazulis.lt/cod-secondary/cif/4/31/56/4315692.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_4315692
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 Gd H2 O2'
_chemical_formula_weight         226.72
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_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                 111.597(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.1490(9)
_cell_length_b                   3.7516(5)
_cell_length_c                   6.7114(9)
_cell_measurement_temperature    141(1)
_cell_volume                     143.95(3)
_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      141(1)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.934
_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  0.0442
_diffrn_reflns_av_sigmaI/netI    0.0245
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            1597
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.72
_diffrn_reflns_theta_min         3.26
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    23.680
_exptl_absorpt_correction_T_max  0.6488
_exptl_absorpt_correction_T_min  0.1633
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.03 (Sheldrick, 2001)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    5.230
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             198
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.624
_refine_diff_density_min         -2.303
_refine_diff_density_rms         0.438
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.493
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     25
_refine_ls_number_reflns         398
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.493
_refine_ls_R_factor_all          0.0271
_refine_ls_R_factor_gt           0.0261
_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^)+(0.0330P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0651
_refine_ls_wR_factor_ref         0.0654
_reflns_number_gt                385
_reflns_number_total             398
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901617c_si_007_03.cif
_cod_data_source_block           apx123me
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_original_formula_sum        'H2 Cl Gd O2'
_cod_database_code               4315692
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'
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
Gd1 Gd 0.30409(6) 0.2500 0.12763(6) 0.00401(19) Uani 1 2 d S . .
Cl1 Cl 0.2457(4) 0.7500 0.4375(3) 0.0068(4) Uani 1 2 d S . .
O1 O 0.0993(11) 0.7500 -0.0825(10) 0.0068(12) Uani 1 2 d S . .
H1 H 0.1155 0.7500 -0.2224 0.008 Uiso 1 2 calc SR . .
O2 O 0.5663(10) 0.7500 0.1619(9) 0.0069(12) Uani 1 2 d S . .
H2 H 0.6971 0.7500 0.3004 0.008 Uiso 1 2 calc SR . .
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
Gd1 0.0014(3) 0.0062(3) 0.0054(3) 0.000 0.00241(18) 0.000
Cl1 0.0045(8) 0.0095(9) 0.0070(9) 0.000 0.0027(7) 0.000
O1 0.006(3) 0.009(3) 0.006(3) 0.000 0.003(2) 0.000
O2 0.004(3) 0.009(3) 0.006(3) 0.000 0.001(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'
Gd Gd -0.1653 3.9035 '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 Gd1 O1 123.1(2) 3_665 3_565 ?
O2 Gd1 O1 77.26(16) 3_665 1_545 ?
O1 Gd1 O1 68.28(17) 3_565 1_545 ?
O2 Gd1 O1 77.26(16) 3_665 . ?
O1 Gd1 O1 68.28(17) 3_565 . ?
O1 Gd1 O1 102.5(2) 1_545 . ?
O2 Gd1 O2 70.35(17) 3_665 . ?
O1 Gd1 O2 129.43(10) 3_565 . ?
O1 Gd1 O2 147.6(2) 1_545 . ?
O1 Gd1 O2 68.86(17) . . ?
O2 Gd1 O2 70.35(17) 3_665 1_545 ?
O1 Gd1 O2 129.43(10) 3_565 1_545 ?
O1 Gd1 O2 68.86(17) 1_545 1_545 ?
O1 Gd1 O2 147.6(2) . 1_545 ?
O2 Gd1 O2 101.1(2) . 1_545 ?
O2 Gd1 Cl1 139.04(4) 3_665 . ?
O1 Gd1 Cl1 72.29(11) 3_565 . ?
O1 Gd1 Cl1 138.04(15) 1_545 . ?
O1 Gd1 Cl1 75.01(13) . . ?
O2 Gd1 Cl1 71.80(12) . . ?
O2 Gd1 Cl1 132.87(15) 1_545 . ?
O2 Gd1 Cl1 139.04(4) 3_665 1_545 ?
O1 Gd1 Cl1 72.29(11) 3_565 1_545 ?
O1 Gd1 Cl1 75.01(13) 1_545 1_545 ?
O1 Gd1 Cl1 138.04(15) . 1_545 ?
O2 Gd1 Cl1 132.87(15) . 1_545 ?
O2 Gd1 Cl1 71.80(12) 1_545 1_545 ?
Cl1 Gd1 Cl1 79.97(5) . 1_545 ?
O2 Gd1 Cl1 108.10(15) 3_665 3_666 ?
O1 Gd1 Cl1 128.76(15) 3_565 3_666 ?
O1 Gd1 Cl1 128.71(12) 1_545 3_666 ?
O1 Gd1 Cl1 128.71(11) . 3_666 ?
O2 Gd1 Cl1 65.94(13) . 3_666 ?
O2 Gd1 Cl1 65.94(13) 1_545 3_666 ?
Cl1 Gd1 Cl1 69.02(5) . 3_666 ?
Cl1 Gd1 Cl1 69.02(5) 1_545 3_666 ?
O2 Gd1 Gd1 90.0 3_665 1_545 ?
O1 Gd1 Gd1 90.000(1) 3_565 1_545 ?
O1 Gd1 Gd1 38.75(11) 1_545 1_545 ?
O1 Gd1 Gd1 141.25(11) . 1_545 ?
O2 Gd1 Gd1 140.56(10) . 1_545 ?
O2 Gd1 Gd1 39.44(10) 1_545 1_545 ?
Cl1 Gd1 Gd1 129.99(3) . 1_545 ?
Cl1 Gd1 Gd1 50.01(3) 1_545 1_545 ?
Cl1 Gd1 Gd1 90.0 3_666 1_545 ?
O2 Gd1 Gd1 90.0 3_665 1_565 ?
O1 Gd1 Gd1 90.0 3_565 1_565 ?
O1 Gd1 Gd1 141.25(11) 1_545 1_565 ?
O1 Gd1 Gd1 38.75(11) . 1_565 ?
O2 Gd1 Gd1 39.44(10) . 1_565 ?
O2 Gd1 Gd1 140.56(10) 1_545 1_565 ?
Cl1 Gd1 Gd1 50.01(3) . 1_565 ?
Cl1 Gd1 Gd1 129.99(3) 1_545 1_565 ?
Cl1 Gd1 Gd1 90.0 3_666 1_565 ?
Gd1 Gd1 Gd1 180.0 1_545 1_565 ?
O2 Gd1 Gd1 35.79(8) 3_665 3_665 ?
O1 Gd1 Gd1 136.36(10) 3_565 3_665 ?
O1 Gd1 Gd1 113.03(14) 1_545 3_665 ?
O1 Gd1 Gd1 69.10(14) . 3_665 ?
O2 Gd1 Gd1 34.56(13) . 3_665 ?
O2 Gd1 Gd1 85.26(11) 1_545 3_665 ?
Cl1 Gd1 Gd1 105.12(3) . 3_665 ?
Cl1 Gd1 Gd1 151.32(4) 1_545 3_665 ?
Cl1 Gd1 Gd1 86.21(3) 3_666 3_665 ?
Gd1 Gd1 Gd1 118.660(7) 1_545 3_665 ?
Gd1 Gd1 Gd1 61.340(6) 1_565 3_665 ?
Gd1 Cl1 Gd1 79.97(5) . 1_565 ?
Gd1 Cl1 Gd1 110.98(5) . 3_666 ?
Gd1 Cl1 Gd1 110.98(5) 1_565 3_666 ?
Gd1 O1 Gd1 111.72(17) 3_565 1_565 ?
Gd1 O1 Gd1 111.72(17) 3_565 . ?
Gd1 O1 Gd1 102.5(2) 1_565 . ?
Gd1 O2 Gd1 109.65(17) 3_665 . ?
Gd1 O2 Gd1 109.65(17) 3_665 1_565 ?
Gd1 O2 Gd1 101.1(2) . 1_565 ?
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
Gd1 O2 2.356(6) 3_665 ?
Gd1 O1 2.385(6) 3_565 ?
Gd1 O1 2.405(4) 1_545 ?
Gd1 O1 2.405(4) . ?
Gd1 O2 2.429(4) . ?
Gd1 O2 2.429(4) 1_545 ?
Gd1 Cl1 2.9190(15) . ?
Gd1 Cl1 2.9191(15) 1_545 ?
Gd1 Cl1 3.199(2) 3_666 ?
Gd1 Gd1 3.7516(5) 1_545 ?
Gd1 Gd1 3.7516(5) 1_565 ?
Gd1 Gd1 3.9111(7) 3_665 ?
Cl1 Gd1 2.9190(15) 1_565 ?
Cl1 Gd1 3.199(2) 3_666 ?
O1 Gd1 2.385(6) 3_565 ?
O1 Gd1 2.405(4) 1_565 ?
O2 Gd1 2.356(6) 3_665 ?
O2 Gd1 2.429(4) 1_565 ?
