#------------------------------------------------------------------------------
#$Date: 2020-03-18 10:18:52 +0200 (Wed, 18 Mar 2020) $
#$Revision: 249481 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/27/7702751.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_7702751
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 H32 Cl6 Gd2 O28'
_chemical_formula_weight         1223.65
_chemical_name_systematic
; 
hexaaquatris(chloranilato)digadolinium(III) hydrate  
;
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                76.90(1)
_cell_angle_beta                 77.15(1)
_cell_angle_gamma                74.79(1)
_cell_formula_units_Z            1
_cell_length_a                   9.381(1)
_cell_length_b                   9.941(1)
_cell_length_c                   11.311(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17.3
_cell_measurement_theta_min      9.6
_cell_volume                     976.37(17)
_computing_cell_refinement       'CAD4 software'
_computing_data_collection       'CAD4 software'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       '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  0.0185
_diffrn_reflns_av_sigmaI/netI    0.0325
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4318
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         1.88
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.872
_exptl_absorpt_correction_T_max  0.9165
_exptl_absorpt_correction_T_min  0.6173
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SHELX-76 (Sheldrick, 1976)'
_exptl_crystal_colour            'deep purple'
_exptl_crystal_density_diffrn    2.081
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'hexagonal prism'
_exptl_crystal_F_000             594
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.764
_refine_diff_density_min         -0.603
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.082
_refine_ls_goodness_of_fit_obs   1.095
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         3567
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.081
_refine_ls_restrained_S_obs      1.094
_refine_ls_R_factor_all          0.0297
_refine_ls_R_factor_obs          0.0235
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0325P)²+0.0555P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0586
_refine_ls_wR_factor_obs         0.0559
_reflns_number_observed          3202
_reflns_number_total             3567
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b109296k.txt
_cod_data_source_block           gdcanabs93
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

data item '_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0325P)^2^+0.0555P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. A new data item '_refine_ls_weighting_details' was
created with the value set to
'w=1/[\s^2^(Fo^2^)+(0.0325P)^2^+0.0555P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        976.4(2)
_cod_database_code               7702751
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
Gd Gd 0.23659(2) 0.33894(2) 0.31586(2) 0.01598(7) Uani 1 d .
O1 O 0.2281(3) 0.0884(3) 0.3422(3) 0.0261(6) Uani 1 d .
O2 O 0.0424(3) 0.2639(3) 0.4777(3) 0.0262(6) Uani 1 d .
C1 C 0.1257(4) 0.0405(4) 0.4142(3) 0.0199(8) Uani 1 d .
C2 C 0.0139(5) 0.1427(4) 0.4919(3) 0.0200(8) Uani 1 d .
C3 C 0.1052(5) -0.0976(4) 0.4281(4) 0.0254(9) Uani 1 d .
Cl1 Cl 0.23332(14) -0.21178(12) 0.34073(12) 0.0412(3) Uani 1 d .
O3 O 0.2179(3) 0.5056(3) 0.1179(2) 0.0234(6) Uani 1 d .
O4 O 0.0559(3) 0.3155(3) 0.2057(3) 0.0283(7) Uani 1 d .
C4 C 0.1173(4) 0.5111(4) 0.0592(3) 0.0198(8) Uani 1 d .
C5 C 0.0249(5) 0.3978(4) 0.1079(3) 0.0210(8) Uani 1 d .
C6 C -0.0837(5) 0.3904(4) 0.0452(4) 0.0233(9) Uani 1 d .
Cl2 Cl -0.18851(15) 0.26309(13) 0.10614(11) 0.0418(3) Uani 1 d .
O5 O 0.2485(3) 0.4189(3) 0.5026(2) 0.0230(6) Uani 1 d .
O6 O 0.4217(3) 0.4778(3) 0.2916(2) 0.0219(6) Uani 1 d .
C7 C 0.3651(4) 0.4554(4) 0.5076(4) 0.0183(8) Uani 1 d .
C8 C 0.4648(4) 0.4912(4) 0.3848(3) 0.0177(8) Uani 1 d .
C9 C 0.4068(4) 0.4636(4) 0.6166(3) 0.0206(8) Uani 1 d .
Cl3 Cl 0.29423(12) 0.41658(13) 0.75523(9) 0.0328(2) Uani 1 d .
O7 O 0.0350(4) 0.5540(3) 0.3437(3) 0.0254(6) Uani 1 d D
H71 H -0.0427(41) 0.5396(58) 0.3710(49) 0.044(17) Uiso 1 d D
H72 H 0.0439(74) 0.5824(63) 0.3989(42) 0.060(20) Uiso 1 d D
O8 O 0.4127(4) 0.2298(4) 0.1597(3) 0.0369(8) Uani 1 d D
H81 H 0.4404(61) 0.2699(52) 0.0956(33) 0.044(16) Uiso 1 d D
H82 H 0.4546(102) 0.1540(47) 0.1780(87) 0.139(41) Uiso 1 d D
O9 O 0.4427(5) 0.1852(4) 0.4220(3) 0.0359(8) Uani 1 d D
H91 H 0.4978(74) 0.1286(64) 0.3878(64) 0.090(28) Uiso 1 d D
H92 H 0.4151(88) 0.1472(74) 0.4857(39) 0.090(29) Uiso 1 d D
O10 O 0.4440(4) 0.6779(4) 0.0673(3) 0.0502(10) Uani 1 d .
O11 O 0.3635(6) 0.0579(4) 0.6673(4) 0.082(2) Uani 1 d .
O12A O 0.4803(22) 0.0588(7) 0.8646(7) 0.068(4) Uani 0.80(4) d P
O12B O 0.5575(52) 0.0671(28) 0.8875(34) 0.053(11) Uani 0.20(4) d P
O13 O 0.0656(7) 0.1379(6) 0.8223(5) 0.091(2) Uani 1 d .
O14A O 0.2059(69) 0.0632(84) 0.0376(53) 0.079(12) Uani 0.37(18) d P
O14B O 0.1549(107) 0.0461(28) 0.0757(85) 0.099(15) Uani 0.63(18) 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'
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
O8 Gd O4 83.53(12) . .
O8 Gd O2 134.14(10) . .
O4 Gd O2 76.51(10) . .
O8 Gd O6 83.09(11) . .
O4 Gd O6 139.11(9) . .
O2 Gd O6 136.69(9) . .
O8 Gd O5 136.07(12) . .
O4 Gd O5 140.31(10) . .
O2 Gd O5 72.01(9) . .
O6 Gd O5 64.77(9) . .
O8 Gd O1 69.48(11) . .
O4 Gd O1 69.64(10) . .
O2 Gd O1 64.95(9) . .
O6 Gd O1 138.33(10) . .
O5 Gd O1 115.71(9) . .
O8 Gd O3 72.51(11) . .
O4 Gd O3 64.92(9) . .
O2 Gd O3 130.32(10) . .
O6 Gd O3 74.22(9) . .
O5 Gd O3 121.44(9) . .
O1 Gd O3 122.74(9) . .
O8 Gd O7 141.31(11) . .
O4 Gd O7 77.75(11) . .
O2 Gd O7 73.43(10) . .
O6 Gd O7 89.31(10) . .
O5 Gd O7 70.61(10) . .
O1 Gd O7 131.57(10) . .
O3 Gd O7 68.92(10) . .
O8 Gd O9 75.12(13) . .
O4 Gd O9 138.70(11) . .
O2 Gd O9 93.53(12) . .
O6 Gd O9 73.21(11) . .
O5 Gd O9 67.64(11) . .
O1 Gd O9 69.86(11) . .
O3 Gd O9 136.13(12) . .
O7 Gd O9 138.25(11) . .
C1 O1 Gd 121.1(2) . .
C2 O2 Gd 121.6(2) . .
O1 C1 C3 125.1(4) . .
O1 C1 C2 116.0(3) . .
C3 C1 C2 118.9(3) . .
O2 C2 C3 125.4(4) . 2_556
O2 C2 C1 115.4(3) . .
C3 C2 C1 119.2(3) 2_556 .
C2 C3 C1 121.9(4) 2_556 .
C2 C3 Cl1 119.8(3) 2_556 .
C1 C3 Cl1 118.2(3) . .
C4 O3 Gd 119.9(2) . .
C5 O4 Gd 123.3(3) . .
O3 C4 C6 125.9(4) . 2_565
O3 C4 C5 116.2(3) . .
C6 C4 C5 117.9(4) 2_565 .
O4 C5 C6 124.5(4) . .
O4 C5 C4 115.1(3) . .
C6 C5 C4 120.4(3) . .
C5 C6 C4 121.6(4) . 2_565
C5 C6 Cl2 118.6(3) . .
C4 C6 Cl2 119.6(3) 2_565 .
C7 O5 Gd 118.5(2) . .
C8 O6 Gd 119.7(2) . .
O5 C7 C9 124.6(4) . .
O5 C7 C8 115.8(3) . .
C9 C7 C8 119.7(3) . .
O6 C8 C9 125.4(4) . 2_666
O6 C8 C7 115.9(3) . .
C9 C8 C7 118.8(3) 2_666 .
C8 C9 C7 121.5(4) 2_666 .
C8 C9 Cl3 119.9(3) 2_666 .
C7 C9 Cl3 118.6(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Gd O8 2.378(3) .
Gd O4 2.400(3) .
Gd O2 2.415(3) .
Gd O6 2.423(3) .
Gd O5 2.453(3) .
Gd O1 2.461(3) .
Gd O3 2.476(3) .
Gd O7 2.483(3) .
Gd O9 2.484(3) .
O1 C1 1.236(5) .
O2 C2 1.269(5) .
C1 C3 1.405(5) .
C1 C2 1.530(5) .
C2 C3 1.378(6) 2_556
C3 C2 1.378(6) 2_556
C3 Cl1 1.725(4) .
O3 C4 1.252(5) .
O4 C5 1.259(5) .
C4 C6 1.390(5) 2_565
C4 C5 1.531(5) .
C5 C6 1.389(6) .
C6 C4 1.390(5) 2_565
C6 Cl2 1.732(4) .
O5 C7 1.256(5) .
O6 C8 1.255(5) .
C7 C9 1.399(5) .
C7 C8 1.518(5) .
C8 C9 1.387(5) 2_666
C9 C8 1.387(5) 2_666
C9 Cl3 1.727(4) .
