#------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/51/29/1512924.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_1512924
loop_
_publ_author_name
'Timothy J. Boyle'
'Leigh Anna M. Ottley'
'Todd M. Alam'
'Mark A. Rodriguez'
'Pin Yang'
'Sarah K. Mcintyre'
_publ_section_title
;
 Structural characterization of methanol substituted lanthanum halides
;
_journal_issue                   7
_journal_name_full               Polyhedron
_journal_page_first              1784
_journal_page_last               1795
_journal_paper_doi               10.1016/j.poly.2010.02.027
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C2 H22 Br3 La O9'
_chemical_formula_weight         568.84
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c 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            8
_cell_length_a                   12.6540(13)
_cell_length_b                   12.9686(13)
_cell_length_c                   19.864(2)
_cell_measurement_temperature    173(2)
_cell_volume                     3259.8(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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    0.0174
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18680
_diffrn_reflns_theta_full        23.27
_diffrn_reflns_theta_max         23.27
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    9.996
_exptl_absorpt_correction_T_max  0.151
_exptl_absorpt_correction_T_min  0.089
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.318
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Irregular
_exptl_crystal_F_000             2144
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.333
_refine_diff_density_min         -0.596
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     224
_refine_ls_number_reflns         2345
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0194
_refine_ls_R_factor_gt           0.0158
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0152P)²+1.7201P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0333
_refine_ls_wR_factor_ref         0.0344
_reflns_number_gt                2120
_reflns_number_total             2345
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            2010-1784.cif
_cod_data_source_block           7sp281s
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        3259.7(6)
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               1512924
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, 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
La1 La 1.013627(13) 0.779404(13) 0.371779(8) 0.01369(7) Uani 1 1 d
Br2 Br 0.74238(2) 0.52228(2) 0.264934(16) 0.02301(9) Uani 1 1 d
Br3 Br 0.06107(3) 0.20246(2) 0.376371(15) 0.02225(9) Uani 1 1 d
Br1 Br 0.77159(2) 0.51539(2) 0.495983(15) 0.02159(9) Uani 1 1 d
O3 O 0.9813(2) 0.9637(2) 0.33487(14) 0.0346(7) Uani 1 1 d
O9 O 0.95145(19) 0.59816(17) 0.34249(12) 0.0249(6) Uani 1 1 d
O7 O 1.1743(2) 0.6767(2) 0.40330(14) 0.0268(6) Uani 1 1 d
O2 O 0.83021(18) 0.8260(2) 0.41205(12) 0.0264(6) Uani 1 1 d
O8 O 0.9770(2) 0.6683(2) 0.47662(13) 0.0246(6) Uani 1 1 d
O5 O 1.18517(19) 0.88178(19) 0.36323(14) 0.0251(6) Uani 1 1 d
O1 O 0.8770(2) 0.7843(2) 0.27537(12) 0.0241(6) Uani 1 1 d
O4 O 1.0379(2) 0.88357(19) 0.47886(13) 0.0266(6) Uani 1 1 d
O6 O 1.1043(2) 0.7378(2) 0.25898(13) 0.0257(6) Uani 1 1 d
C1 C 0.9939(3) 0.4973(3) 0.3569(2) 0.0290(9) Uani 1 1 d
C2 C 0.7318(3) 0.7717(3) 0.4068(2) 0.0321(9) Uani 1 1 d
H9 H 1.195(2) 0.912(2) 0.3346(16) 0.011(10) Uiso 1 1 d
H16 H 0.745(3) 0.703(3) 0.3888(17) 0.044(11) Uiso 1 1 d
H7 H 1.089(3) 0.911(3) 0.4867(18) 0.044(14) Uiso 1 1 d
H3 H 0.977(2) 0.691(2) 0.5080(15) 0.006(10) Uiso 1 1 d
H14 H 0.880(3) 0.755(3) 0.237(2) 0.050(13) Uiso 1 1 d
H10 H 1.010(3) 1.015(3) 0.347(2) 0.047(14) Uiso 1 1 d
H15 H 0.839(3) 0.824(3) 0.2742(16) 0.018(11) Uiso 1 1 d
H6 H 1.009(3) 0.877(3) 0.5128(18) 0.039(13) Uiso 1 1 d
H2 H 0.924(3) 0.627(3) 0.4743(19) 0.060(14) Uiso 1 1 d
H18 H 0.683(3) 0.814(3) 0.379(2) 0.073(15) Uiso 1 1 d
H11 H 0.925(3) 0.984(3) 0.324(2) 0.063(16) Uiso 1 1 d
H17 H 0.700(4) 0.762(3) 0.452(2) 0.082(16) Uiso 1 1 d
H8 H 1.221(3) 0.908(3) 0.397(2) 0.065(15) Uiso 1 1 d
H12 H 1.146(3) 0.693(3) 0.2561(19) 0.047(14) Uiso 1 1 d
H5 H 1.231(3) 0.691(3) 0.3937(18) 0.036(13) Uiso 1 1 d
H4 H 1.178(3) 0.634(4) 0.430(2) 0.070(18) Uiso 1 1 d
H13 H 1.071(4) 0.735(3) 0.227(2) 0.067(18) Uiso 1 1 d
H21 H 1.064(4) 0.509(3) 0.366(2) 0.073(16) Uiso 1 1 d
H22 H 0.987(4) 0.451(4) 0.318(3) 0.107(19) Uiso 1 1 d
H23 H 0.954(4) 0.468(4) 0.386(2) 0.094(19) Uiso 1 1 d
H25 H 0.900(3) 0.593(3) 0.3253(17) 0.034(12) Uiso 1 1 d
H24 H 0.821(2) 0.872(2) 0.4276(15) 0.010(10) Uiso 1 1 d
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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
O7 La1 O2 142.32(9)
O7 La1 O3 134.72(10)
O2 La1 O3 73.62(9)
O7 La1 O4 88.58(8)
O2 La1 O4 73.68(9)
O3 La1 O4 76.11(9)
O7 La1 O9 79.49(8)
O2 La1 O9 90.52(8)
O3 La1 O9 139.02(9)
O4 La1 O9 136.07(8)
O7 La1 O5 66.63(9)
O2 La1 O5 132.70(8)
O3 La1 O5 68.10(9)
O4 La1 O5 71.07(9)
O9 La1 O5 136.76(8)
O7 La1 O6 75.22(9)
O2 La1 O6 137.27(9)
O3 La1 O6 91.01(9)
O4 La1 O6 141.88(9)
O9 La1 O6 75.26(8)
O5 La1 O6 70.83(8)
O7 La1 O8 69.33(9)
O2 La1 O8 73.29(8)
O3 La1 O8 137.14(9)
O4 La1 O8 69.01(9)
O9 La1 O8 67.20(9)
O5 La1 O8 119.90(9)
O6 La1 O8 131.84(9)
O7 La1 O1 137.81(9)
O2 La1 O1 67.29(8)
O3 La1 O1 69.75(9)
O4 La1 O1 133.62(9)
O9 La1 O1 69.27(8)
O5 La1 O1 120.53(8)
O6 La1 O1 70.00(9)
O8 La1 O1 119.56(8)
La1 O3 H10 129(3)
La1 O3 H11 123(3)
H10 O3 H11 102(4)
C1 O9 La1 132.6(2)
C1 O9 H25 110(3)
La1 O9 H25 117(3)
La1 O7 H5 125(3)
La1 O7 H4 127(3)
H5 O7 H4 107(4)
C2 O2 La1 131.1(2)
C2 O2 H24 109(3)
La1 O2 H24 120(3)
La1 O8 H3 120(3)
La1 O8 H2 117(3)
H3 O8 H2 108(4)
La1 O5 H9 120(3)
La1 O5 H8 127(3)
H9 O5 H8 107(4)
La1 O1 H14 128(3)
La1 O1 H15 120(3)
H14 O1 H15 109(4)
La1 O4 H7 122(3)
La1 O4 H6 128(3)
H7 O4 H6 106(4)
La1 O6 H12 121(3)
La1 O6 H13 119(3)
H12 O6 H13 106(4)
O9 C1 H21 104(3)
O9 C1 H22 111(3)
H21 C1 H22 110(3)
O9 C1 H23 108(3)
H21 C1 H23 121(4)
H22 C1 H23 103(4)
O2 C2 H16 109(2)
O2 C2 H18 108(2)
H16 C2 H18 115(3)
O2 C2 H17 110(3)
H16 C2 H17 107(3)
H18 C2 H17 108(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
La1 O7 2.510(2)
La1 O2 2.528(2)
La1 O3 2.533(3)
La1 O4 2.538(2)
La1 O9 2.546(2)
La1 O5 2.550(2)
La1 O6 2.575(2)
La1 O8 2.575(2)
La1 O1 2.581(2)
O3 H10 0.80(4)
O3 H11 0.79(4)
O9 C1 1.442(4)
O9 H25 0.74(3)
O7 H5 0.76(4)
O7 H4 0.76(4)
O2 C2 1.434(4)
O2 H24 0.69(3)
O8 H3 0.69(3)
O8 H2 0.86(4)
O5 H9 0.70(3)
O5 H8 0.87(4)
O1 H14 0.85(4)
O1 H15 0.70(3)
O4 H7 0.76(4)
O4 H6 0.77(4)
O6 H12 0.79(4)
O6 H13 0.76(4)
C1 H21 0.92(5)
C1 H22 0.99(5)
C1 H23 0.85(5)
C2 H16 0.98(4)
C2 H18 0.99(4)
C2 H17 0.99(5)
