#------------------------------------------------------------------------------
#$Date: 2019-11-28 15:00:32 +0200 (Thu, 28 Nov 2019) $
#$Revision: 243998 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/27/7702752.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_7702752
loop_
_publ_author_name
'Abrahams, Brendan F.'
'Coleiro, Joseph'
'Ha, Karen'
'Hoskins, Bernard F.'
'Orchard, Simon D.'
'Robson, Richard'
_publ_section_title
;
 Dihydroxybenzoquinone and chloranilic acid derivatives of rare earth
 metals
;
_journal_issue                   8
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1586
_journal_paper_doi               10.1039/b109296k
_journal_year                    2002
_chemical_formula_sum            'C18 H24 Cl6 Lu2 O24'
_chemical_formula_weight         1187.01
_chemical_name_systematic
; 
octaaquatris(chloranilato)dilutetium(III) hydrate 
;
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.97(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.956(8)
_cell_length_b                   16.680(5)
_cell_length_c                   10.970(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13.3
_cell_measurement_theta_min      7.1
_cell_volume                     3239(2)
_computing_cell_refinement       'CAD4 - Software'
_computing_data_collection       'CAD4 - Software'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Enraf-Nonius CAD4 diffractometer'
_diffrn_measurement_method       ω:2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0782
_diffrn_reflns_av_sigmaI/netI    0.1403
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            3647
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         1.99
_diffrn_standards_decay_%        3
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.653
_exptl_absorpt_correction_T_max  0.9099
_exptl_absorpt_correction_T_min  0.6196
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SHELX-76 (Sheldrick, 1976)'
_exptl_crystal_colour            'deep purple'
_exptl_crystal_density_diffrn    2.434
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular plate'
_exptl_crystal_F_000             2272
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.014
_refine_diff_density_max         3.910
_refine_diff_density_min         -3.714
_refine_diff_density_rms         0.489
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     198
_refine_ls_number_reflns         2915
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1557
_refine_ls_R_factor_gt           0.0859
_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)+(0.1190P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1932
_refine_ls_wR_factor_ref         0.2303
_reflns_number_gt                1678
_reflns_number_total             2915
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b109296k.txt
_cod_data_source_block           lucanabs97
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               7702752
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z'
'-x, -y, -z'
'-x, y, -z'
'-x+1/2, -y+1/2, -z'
'-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
_atom_site_refinement_flags
Lu1 Lu 0.11592(8) 0.5000 -0.18417(15) 0.0200(4) Uani 1 2 d S
Cl1 Cl 0.3390(3) 0.3107(4) -0.1821(7) 0.0315(15) Uani 1 1 d .
Cl2 Cl 0.0246(4) 0.7958(4) -0.1540(9) 0.044(2) Uani 1 1 d .
O1 O 0.2033(8) 0.4118(9) -0.2102(18) 0.025(4) Uani 1 1 d .
O2 O 0.0806(9) 0.6296(9) -0.1817(17) 0.029(4) Uani 1 1 d .
C1 C 0.2006(13) 0.3374(14) -0.188(2) 0.021(5) Uiso 1 1 d .
C2 C 0.1227(14) 0.6865(16) -0.175(3) 0.029(6) Uiso 1 1 d .
C3 C 0.1088(14) 0.7658(14) -0.167(3) 0.027(6) Uiso 1 1 d .
C4 C 0.1644(13) 0.1727(14) -0.152(2) 0.024(5) Uiso 1 1 d .
C5 C 0.2428(13) 0.1977(13) -0.159(2) 0.018(5) Uiso 1 1 d .
C6 C 0.2539(15) 0.2797(15) -0.173(3) 0.031(6) Uiso 1 1 d .
O3 O 0.1555(10) 0.1017(11) -0.1360(19) 0.036(5) Uani 1 1 d .
O4 O 0.2849(10) 0.1447(9) -0.161(2) 0.041(5) Uani 1 1 d .
O5 O 0.0969(15) 0.5000 -0.408(3) 0.042(7) Uani 1 2 d S
O6 O -0.0215(13) 0.5000 -0.293(3) 0.030(6) Uani 1 2 d S
O7 O 0.0720(12) 0.5000 -0.014(3) 0.031(6) Uani 1 2 d S
O8 O 0.2189(16) 0.5000 0.007(2) 0.039(7) Uani 1 2 d S
Lu2 Lu 0.31037(8) 0.5000 0.50321(15) 0.0208(4) Uani 1 2 d S
Cl3 Cl 0.4142(3) 0.2012(4) 0.5111(7) 0.0321(16) Uani 1 1 d .
O9 O 0.2150(9) 0.4061(8) 0.4989(15) 0.021(4) Uani 1 1 d .
O10 O 0.3462(9) 0.3649(9) 0.5002(19) 0.031(4) Uani 1 1 d .
C7 C 0.2262(12) 0.3329(13) 0.494(2) 0.019(5) Uiso 1 1 d .
C8 C 0.3063(10) 0.3081(11) 0.4996(19) 0.006(4) Uiso 1 1 d .
C9 C 0.3255(12) 0.2265(12) 0.502(2) 0.016(5) Uiso 1 1 d .
O11 O 0.4310(16) 0.5220(19) 0.643(3) 0.033(12) Uani 0.50 1 d P
O12 O 0.3081(12) 0.5000 0.712(2) 0.023(5) Uani 1 2 d S
O13 O 0.3845(15) 0.5000 0.374(3) 0.036(6) Uani 1 2 d S
O14 O 0.2296(15) 0.5000 0.294(2) 0.033(6) Uani 1 2 d S
O15 O 0.531(2) 0.5000 0.899(4) 0.091(13) Uiso 1 2 d S
O16 O 0.5000 0.6152(17) 0.5000 0.046(8) Uani 1 2 d S
O17 O 0.4307(9) 0.1186(11) -0.157(2) 0.045(6) Uani 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'
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
O2 Lu1 O2 145.1(8) 2_565 .
O2 Lu1 O8 98.4(4) 2_565 .
O2 Lu1 O8 98.5(4) . .
O2 Lu1 O7 78.2(5) 2_565 .
O2 Lu1 O7 78.2(5) . .
O8 Lu1 O7 72.3(9) . .
O2 Lu1 O1 67.8(6) 2_565 .
O2 Lu1 O1 146.9(6) . .
O8 Lu1 O1 72.6(7) . .
O7 Lu1 O1 125.8(5) . .
O2 Lu1 O1 146.9(6) 2_565 2_565
O2 Lu1 O1 67.8(6) . 2_565
O8 Lu1 O1 72.6(7) . 2_565
O7 Lu1 O1 125.8(5) . 2_565
O1 Lu1 O1 79.2(7) . 2_565
O2 Lu1 O5 94.4(5) 2_565 .
O2 Lu1 O5 94.4(5) . .
O8 Lu1 O5 135.7(10) . .
O7 Lu1 O5 152.0(9) . .
O1 Lu1 O5 73.7(7) . .
O1 Lu1 O5 73.7(7) 2_565 .
O2 Lu1 O6 74.8(4) 2_565 .
O2 Lu1 O6 74.8(4) . .
O8 Lu1 O6 148.5(10) . .
O7 Lu1 O6 76.2(8) . .
O1 Lu1 O6 128.8(5) . .
O1 Lu1 O6 128.8(5) 2_565 .
O5 Lu1 O6 75.7(9) . .
C1 O1 Lu1 121.4(14) . .
C2 O2 Lu1 123.4(16) . .
O1 C1 C6 130(2) . .
O1 C1 C2 111(2) . 2_565
C6 C1 C2 119(2) . 2_565
O2 C2 C3 128(2) . .
O2 C2 C1 114(2) . 2_565
C3 C2 C1 117(2) . 2_565
C2 C3 C4 123(2) . 2_565
C2 C3 Cl2 119.7(19) . .
C4 C3 Cl2 116.5(18) 2_565 .
O3 C4 C3 125(2) . 2_565
O3 C4 C5 117(2) . .
C3 C4 C5 118(2) 2_565 .
O4 C5 C6 126(2) . .
O4 C5 C4 117(2) . .
C6 C5 C4 117(2) . .
C1 C6 C5 125(2) . .
C1 C6 Cl1 116.6(19) . .
C5 C6 Cl1 118.5(19) . .
O14 Lu2 O11 146.7(11) . .
O14 Lu2 O11 146.7(11) . 2_565
O11 Lu2 O11 18.5(16) . 2_565
O14 Lu2 O12 139.7(9) . .
O11 Lu2 O12 72.6(10) . .
O11 Lu2 O12 72.6(10) 2_565 .
O14 Lu2 O13 73.6(10) . .
O11 Lu2 O13 74.5(11) . .
O11 Lu2 O13 74.5(11) 2_565 .
O12 Lu2 O13 146.7(8) . .
O14 Lu2 O10 94.6(5) . 2_565
O11 Lu2 O10 68.4(9) . 2_565
O11 Lu2 O10 86.5(9) 2_565 2_565
O12 Lu2 O10 97.0(5) . 2_565
O13 Lu2 O10 75.6(4) . 2_565
O14 Lu2 O10 94.6(5) . .
O11 Lu2 O10 86.5(9) . .
O11 Lu2 O10 68.4(9) 2_565 .
O12 Lu2 O10 97.0(5) . .
O13 Lu2 O10 75.6(4) . .
O10 Lu2 O10 145.9(8) 2_565 .
O14 Lu2 O9 75.3(6) . 2_565
O11 Lu2 O9 118.6(9) . 2_565
O11 Lu2 O9 133.6(9) 2_565 2_565
O12 Lu2 O9 74.7(5) . 2_565
O13 Lu2 O9 127.4(5) . 2_565
O10 Lu2 O9 65.8(5) 2_565 2_565
O10 Lu2 O9 148.2(5) . 2_565
O14 Lu2 O9 75.3(7) . .
O11 Lu2 O9 133.6(9) . .
O11 Lu2 O9 118.6(9) 2_565 .
O12 Lu2 O9 74.7(5) . .
O13 Lu2 O9 127.4(5) . .
O10 Lu2 O9 148.2(5) 2_565 .
O10 Lu2 O9 65.8(5) . .
O9 Lu2 O9 82.4(7) 2_565 .
C7 O9 Lu2 120.6(14) . .
C8 O10 Lu2 124.5(13) . .
O9 C7 C9 124(2) . 7_556
O9 C7 C8 116.0(19) . .
C9 C7 C8 119.6(19) 7_556 .
O10 C8 C9 126.8(18) . .
O10 C8 C7 113.0(17) . .
C9 C8 C7 120.2(17) . .
C7 C9 C8 120(2) 7_556 .
C7 C9 Cl3 120.5(17) 7_556 .
C8 C9 Cl3 119.1(16) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Lu1 O2 2.266(15) 2_565
Lu1 O2 2.266(15) .
Lu1 O8 2.30(3) .
Lu1 O7 2.30(2) .
Lu1 O1 2.308(15) .
Lu1 O1 2.308(15) 2_565
Lu1 O5 2.35(3) .
Lu1 O6 2.45(2) .
Cl1 C6 1.73(3) .
Cl2 C3 1.73(2) .
O1 C1 1.27(3) .
O2 C2 1.23(3) .
C1 C6 1.36(3) .
C1 C2 1.58(3) 2_565
C2 C3 1.36(4) .
C2 C1 1.58(3) 2_565
C3 C4 1.44(3) 2_565
C4 O3 1.22(3) .
C4 C3 1.44(3) 2_565
C4 C5 1.57(3) .
C5 O4 1.20(3) .
C5 C6 1.40(3) .
Lu2 O14 2.26(2) .
Lu2 O11 2.28(3) .
Lu2 O11 2.28(3) 2_565
Lu2 O12 2.31(2) .
Lu2 O13 2.33(3) .
Lu2 O10 2.357(15) 2_565
Lu2 O10 2.357(15) .
Lu2 O9 2.379(14) 2_565
Lu2 O9 2.380(14) .
Cl3 C9 1.70(2) .
O9 C7 1.24(3) .
O10 C8 1.21(2) .
C7 C9 1.41(3) 7_556
C7 C8 1.55(3) .
C8 C9 1.41(3) .
C9 C7 1.41(3) 7_556
