#------------------------------------------------------------------------------
#$Date: 2019-11-28 15:00:32 +0200 (Thu, 28 Nov 2019) $
#$Revision: 243998 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/27/7702749.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_7702749
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 H36 Ce2 Cl6 O30'
_chemical_formula_weight         1225.41
_chemical_name_systematic
; 
hexaaquatris(chloranilato)dicerium(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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.83(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.376(2)
_cell_length_b                   16.598(3)
_cell_length_c                   11.224(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15.4
_cell_measurement_theta_min      7.7
_cell_volume                     2116.7(7)
_computing_cell_refinement       'CAD4 - Software'
_computing_data_collection       'CAD4 - Software'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0155
_diffrn_reflns_av_sigmaI/netI    0.0305
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            3084
_diffrn_reflns_theta_full        27.55
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         1.82
_diffrn_standards_decay_%        6
_diffrn_standards_interval_time  160
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.596
_exptl_absorpt_correction_T_max  0.8025
_exptl_absorpt_correction_T_min  0.5931
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SHELX-76 (Sheldrick, 1976)'
_exptl_crystal_colour            'deep purple'
_exptl_crystal_density_diffrn    1.923
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular prism'
_exptl_crystal_F_000             1204
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.907
_refine_diff_density_min         -0.874
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         2513
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0340
_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)+(0.0537P)²+4.1500P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0899
_refine_ls_wR_factor_ref         0.0939
_reflns_number_gt                2204
_reflns_number_total             2513
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b109296k.txt
_cod_data_source_block           cecanabs97
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7702749
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
Ce1 Ce 0.28350(3) 0.0000 0.15605(3) 0.02447(11) Uani 1 2 d S
Cl1 Cl 0.44135(11) 0.20515(7) -0.18610(12) 0.0463(3) Uani 1 1 d .
O1 O 0.3453(3) 0.10136(18) 0.0042(3) 0.0327(7) Uani 1 1 d .
O2 O 0.1856(3) 0.13780(18) 0.1559(3) 0.0364(7) Uani 1 1 d .
C1 C 0.3050(3) 0.1717(2) -0.0032(4) 0.0272(8) Uani 1 1 d .
C2 C 0.2121(3) 0.1929(2) 0.0860(4) 0.0285(8) Uani 1 1 d .
C3 C 0.3379(4) 0.2297(3) -0.0841(4) 0.0317(9) Uani 1 1 d .
Cl2 Cl 0.5000 0.19069(9) 0.5000 0.0456(4) Uani 1 2 d S
O3 O 0.3727(3) 0.07901(18) 0.3284(3) 0.0341(7) Uani 1 1 d .
C4 C 0.4342(3) 0.0462(2) 0.4115(4) 0.0277(8) Uani 1 1 d .
C5 C 0.5000 0.0870(4) 0.5000 0.0306(12) Uani 1 2 d S
O4 O 0.5127(4) 0.0000 0.1426(4) 0.0355(10) Uani 1 2 d S
O5 O 0.1264(5) 0.0000 -0.0130(5) 0.0558(14) Uani 1 2 d S
O6 O 0.1168(5) 0.0000 0.2914(6) 0.0604(15) Uani 1 2 d S
O7 O 0.0805(7) 0.1177(5) 0.8239(9) 0.148(3) Uani 1 1 d .
O8 O 0.2696(13) 0.0000 0.6773(14) 0.100 Uiso 0.580(18) 2 d SP
O9 O 0.2768(12) 0.2945(9) 0.5939(14) 0.100 Uiso 0.439(12) 1 d P
O10 O 0.1985(14) 0.1353(10) 0.6269(15) 0.100 Uiso 0.404(12) 1 d P
O11 O 0.4354(15) 0.3745(12) 0.5840(16) 0.100 Uiso 0.360(12) 1 d P
O12 O 0.217(2) 0.2448(14) 0.651(2) 0.100 Uiso 0.293(12) 1 d P
O13 O 0.335(2) 0.3671(14) 0.507(2) 0.100 Uiso 0.284(11) 1 d P
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'
Ce Ce -0.2486 2.6331 '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
O6 Ce1 O3 79.66(15) . 2
O6 Ce1 O3 79.66(15) . .
O3 Ce1 O3 63.00(13) 2 .
O6 Ce1 O1 131.27(10) . 2
O3 Ce1 O1 93.27(10) 2 2
O3 Ce1 O1 139.01(10) . 2
O6 Ce1 O1 131.27(10) . .
O3 Ce1 O1 139.02(10) 2 .
O3 Ce1 O1 93.27(10) . .
O1 Ce1 O1 83.79(14) 2 .
O6 Ce1 O5 85.8(2) . .
O3 Ce1 O5 144.90(9) 2 .
O3 Ce1 O5 144.90(9) . .
O1 Ce1 O5 72.80(12) 2 .
O1 Ce1 O5 72.80(12) . .
O6 Ce1 O2 69.73(8) . .
O3 Ce1 O2 129.10(10) 2 .
O3 Ce1 O2 72.00(10) . .
O1 Ce1 O2 137.44(10) 2 .
O1 Ce1 O2 62.34(9) . .
O5 Ce1 O2 73.01(9) . .
O6 Ce1 O2 69.73(8) . 2
O3 Ce1 O2 72.00(10) 2 2
O3 Ce1 O2 129.10(10) . 2
O1 Ce1 O2 62.34(9) 2 2
O1 Ce1 O2 137.44(10) . 2
O5 Ce1 O2 73.01(9) . 2
O2 Ce1 O2 128.08(15) . 2
O6 Ce1 O4 145.70(19) . .
O3 Ce1 O4 71.25(12) 2 .
O3 Ce1 O4 71.25(12) . .
O1 Ce1 O4 69.48(10) 2 .
O1 Ce1 O4 69.48(10) . .
O5 Ce1 O4 128.50(18) . .
O2 Ce1 O4 115.91(7) . .
O2 Ce1 O4 115.91(7) 2 .
C1 O1 Ce1 123.6(3) . .
C2 O2 Ce1 122.6(3) . .
O1 C1 C3 125.4(4) . .
O1 C1 C2 115.5(4) . .
C3 C1 C2 119.0(3) . .
O2 C2 C3 124.6(4) . 7
O2 C2 C1 115.9(4) . .
C3 C2 C1 119.5(4) 7 .
C1 C3 C2 121.5(4) . 7
C1 C3 Cl1 118.9(3) . .
C2 C3 Cl1 119.5(3) 7 .
C4 O3 Ce1 122.2(3) . .
O3 C4 C5 125.3(4) . .
O3 C4 C4 115.6(2) . 2
C5 C4 C4 119.1(3) . 2
C4 C5 C4 121.7(5) . 6_656
C4 C5 Cl2 119.1(3) . .
C4 C5 Cl2 119.1(3) 6_656 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ce1 O6 2.488(5) .
Ce1 O3 2.510(3) 2
Ce1 O3 2.510(3) .
Ce1 O1 2.519(3) 2
Ce1 O1 2.519(3) .
Ce1 O5 2.541(5) .
Ce1 O2 2.544(3) .
Ce1 O2 2.544(3) 2
Ce1 O4 2.619(4) .
Cl1 C3 1.731(4) .
O1 C1 1.255(5) .
O2 C2 1.251(5) .
C1 C3 1.387(6) .
C1 C2 1.533(6) .
C2 C3 1.406(6) 7
C3 C2 1.406(6) 7
Cl2 C5 1.721(6) .
O3 C4 1.261(5) .
C4 C5 1.390(5) .
C4 C4 1.534(8) 2
C5 C4 1.390(5) 6_656
