#------------------------------------------------------------------------------
#$Date: 2022-04-22 18:09:36 +0200 (vie 22 de abr de 2022) $
#$Revision: 274638 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/38/7203848.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_7203848
loop_
_publ_author_name
'Umebayashi, Yasuhiro'
'Matsumoto, Kai'
'Mekata, Isamu'
'Ishiguro, Shin-ichi'
_publ_section_title
;
 Solvation structure of lanthanide(iii) ions in solvent mixtures of
 N,N-dimethylformamide and N,N-dimethylacetamide studied by titration
 Raman spectroscopy
;
_journal_coden_ASTM              PPCPFQ
_journal_issue                   22
_journal_name_full               'Physical Chemistry Chemical Physics'
_journal_page_first              5599
_journal_page_last               5605
_journal_paper_doi               10.1039/b204162f
_journal_volume                  4
_journal_year                    2002
_chemical_formula_sum            'C28 H60 Cl3 Gd N8 O20'
_chemical_formula_weight         1092.43
_space_group_IT_number           90
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      90
_symmetry_space_group_name_Hall  'P 4ab 2ab'
_symmetry_space_group_name_H-M   'P 4 21 2'
_cell_angle_alpha                89.99(4)
_cell_angle_beta                 90.02(2)
_cell_angle_gamma                90.00(3)
_cell_formula_units_Z            2
_cell_length_a                   15.501(4)
_cell_length_b                   15.497(8)
_cell_length_c                   10.428(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      11.8
_cell_measurement_theta_min      10.1
_cell_volume                     2505.0(16)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_publication_material  'teXsan Ver. 1.11'
_computing_structure_refinement  'teXsan Ver. 1.10'
_computing_structure_solution    DirectMethod
_diffrn_measured_fraction_theta_full 0.9977
_diffrn_measured_fraction_theta_max 0.9977
_diffrn_measurement_device_type  'Rigaku AFC5S'
_diffrn_measurement_method       ω-2θ
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1713
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_standards_decay_%        0.62
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.560
_exptl_absorpt_correction_T_max  0.998
_exptl_absorpt_correction_T_min  0.886
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.99
_refine_diff_density_min         -1.18
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     168
_refine_ls_number_reflns         1157
_refine_ls_R_factor_gt           0.0442
_refine_ls_shift/su_max          0.4654
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[σ²(Fo) + 0.00302|Fo|²]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0600
_reflns_number_gt                1157
_reflns_number_total             1704
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            185878.cif
_cod_data_source_block           Gd_comp
_cod_original_cell_volume        2504(1)
_cod_original_sg_symbol_H-M      'P 4 21 2     '
_cod_original_formula_sum        'C28 H60 Cl3 Gd N8 O20 '
_cod_database_code               7203848
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,z
1/2-x,1/2+y,-z
1/2+x,1/2-y,-z
y,x,-z
-y,-x,-z
1/2+y,1/2-x,z
1/2-y,1/2+x,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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd Gd 0.0000 0.0000 0.0000 0.04539(10) Uani 1.00 d S . .
Cl(1) Cl 0.2068(2) 0.2068 0.5000 0.0721(4) Uani 1.00 d S . .
Cl(2) Cl 0.5000 0.0000 0.0017(7) 0.0879(8) Uani 1.00 d S . .
O(1) O 0.1368(4) -0.0440(5) -0.0879(6) 0.068(2) Uani 1.00 d . . .
O(2) O 0.1012(4) 0.0380(5) 0.1586(7) 0.071(2) Uani 1.00 d . . .
O(3) O 0.2873(8) 0.195(1) 0.453(2) 0.242(8) Uani 1.00 d . . .
O(4) O 0.1933(8) 0.1453(7) 0.594(1) 0.170(6) Uani 1.00 d . . .
O(5) O 0.5000 0.0000 0.134(2) 0.197(6) Uani 1.00 d S . .
O(6) O 0.451(3) -0.001(9) -0.089(5) 0.26(4) Uani 0.25 d P . .
O(7) O 0.588(2) 0.027(4) -0.013(3) 0.23(2) Uani 0.50 d P . .
N(1) N 0.2540(5) -0.0672(6) -0.2109(8) 0.061(2) Uani 1.00 d . . .
N(2) N 0.210(1) -0.011(1) 0.281(1) 0.050(4) Uani 0.50 d P . .
N(3) N 0.235(1) 0.025(1) 0.224(2) 0.065(6) Uani 0.50 d P . .
C(1) C 0.1882(7) -0.0204(6) -0.1717(9) 0.057(3) Uani 1.00 d . . .
C(2) C 0.2728(9) -0.1499(9) -0.150(2) 0.106(5) Uani 1.00 d . . .
C(3) C 0.3111(8) -0.0367(8) -0.311(1) 0.078(3) Uani 1.00 d . . .
C(4) C 0.179(2) 0.036(2) 0.185(2) 0.056(7) Uani 0.50 d P . .
C(5) C 0.2524(10) 0.088(1) 0.107(2) 0.104(5) Uani 1.00 d . . .
C(6) C 0.3024(8) -0.002(1) 0.313(1) 0.098(4) Uani 1.00 d . . .
C(7) C 0.139(1) -0.0434(9) 0.361(1) 0.099(4) Uani 1.00 d . . .
C(8) C 0.154(2) 0.003(2) 0.240(3) 0.09(1) Uani 0.50 d P . .
H(1) H 0.1783 0.0346 -0.2071 0.0696 Uani 1.00 calc . . .
H(2) H 0.2829 -0.1381 -0.0589 0.1372 Uani 1.00 calc . . .
H(3) H 0.2268 -0.1861 -0.1592 0.1372 Uani 1.00 calc . . .
H(4) H 0.3244 -0.1720 -0.1845 0.1372 Uani 1.00 calc . . .
H(5) H 0.3381 0.0149 -0.2835 0.0958 Uani 1.00 calc . . .
H(6) H 0.2810 -0.0299 -0.3859 0.0958 Uani 1.00 calc . . .
H(7) H 0.3554 -0.0804 -0.3206 0.0958 Uani 1.00 calc . . .
H(8) H 0.3131 -0.0655 0.3125 0.1112 Uani 1.00 calc . . .
H(9) H 0.2941 0.0111 0.4041 0.1112 Uani 1.00 calc . . .
H(10) H 0.3544 0.0240 0.2869 0.1112 Uani 1.00 calc . . .
H(11) H 0.1656 -0.1013 0.3587 0.1239 Uani 0.50 calc P . .
H(12) H 0.1610 -0.0147 0.4329 0.1239 Uani 0.50 calc P . .
H(13) H 0.0779 -0.0544 0.3749 0.1239 Uani 0.50 calc P . .
H(14) H 0.2818 0.1267 0.1634 0.1298 Uani 0.50 calc P . .
H(15) H 0.2276 0.1181 0.0389 0.1298 Uani 0.50 calc P . .
H(16) H 0.2946 0.0476 0.0743 0.1298 Uani 0.50 calc P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.002
;International Tables for Crystallography

(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)

;
H H 0.000 0.000
;International Tables for Crystallography

(1992, Vol. C, Table 6.1.1.2)

;
N N 0.006 0.003
;International Tables for Crystallography

(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)

;
O O 0.011 0.006
;International Tables for Crystallography

(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)

;
Cl Cl 0.148 0.159
;International Tables for Crystallography

(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)

;
Gd Gd -0.165 3.904
;International Tables for Crystallography

(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)

;
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O(1) Gd O(1) 135.3(3) . . 2_555 yes
O(1) Gd O(1) 130.0(3) . . 5_555 yes
O(1) Gd O(1) 69.3(3) . . 6_555 yes
O(1) Gd O(2) 75.6(2) . . . yes
O(1) Gd O(2) 141.6(2) . . 2_555 yes
O(1) Gd O(2) 72.6(2) . . 5_555 yes
O(1) Gd O(2) 76.3(2) . . 6_555 yes
O(1) Gd O(1) 69.3(3) 2_555 . 5_555 yes
O(1) Gd O(1) 130.0(3) 2_555 . 6_555 yes
O(1) Gd O(2) 141.6(2) 2_555 . . yes
O(1) Gd O(2) 75.6(2) 2_555 . 2_555 yes
O(1) Gd O(2) 76.4(2) 2_555 . 5_555 yes
O(1) Gd O(2) 72.6(2) 2_555 . 6_555 yes
O(1) Gd O(1) 135.2(3) 5_555 . 6_555 yes
O(1) Gd O(2) 72.6(2) 5_555 . . yes
O(1) Gd O(2) 76.3(2) 5_555 . 2_555 yes
O(1) Gd O(2) 75.6(2) 5_555 . 5_555 yes
O(1) Gd O(2) 141.6(2) 5_555 . 6_555 yes
O(1) Gd O(2) 76.4(2) 6_555 . . yes
O(1) Gd O(2) 72.6(2) 6_555 . 2_555 yes
O(1) Gd O(2) 141.5(2) 6_555 . 5_555 yes
O(1) Gd O(2) 75.6(2) 6_555 . 6_555 yes
O(2) Gd O(2) 90.7(4) . . 2_555 yes
O(2) Gd O(2) 99.2(4) . . 5_555 yes
O(2) Gd O(2) 145.8(4) . . 6_555 yes
O(2) Gd O(2) 145.8(3) 2_555 . 5_555 yes
O(2) Gd O(2) 99.2(4) 2_555 . 6_555 yes
O(2) Gd O(2) 90.7(4) 5_555 . 6_555 yes
O(3) Cl(1) O(3) 111(1) . . 5_556 yes
O(3) Cl(1) O(4) 108.0(9) . . . yes
O(3) Cl(1) O(4) 110.9(9) . . 5_556 yes
O(3) Cl(1) O(4) 110.9(9) 5_556 . . yes
O(3) Cl(1) O(4) 107.9(9) 5_556 . 5_556 yes
O(4) Cl(1) O(4) 107(1) . . 5_556 yes
O(5) Cl(2) O(6) 141(2) . . . yes
O(5) Cl(2) O(6) 141(2) . . 7_555 yes
O(5) Cl(2) O(6) 141(2) . . 8_545 yes
O(5) Cl(2) O(6) 141(2) . . 2_655 yes
O(5) Cl(2) O(7) 96(1) . . . yes
O(5) Cl(2) O(7) 96(1) . . 7_555 yes
O(5) Cl(2) O(7) 96(1) . . 8_545 yes
O(5) Cl(2) O(7) 96(1) . . 2_655 yes
O(6) Cl(2) O(6) 52(3) . . 7_555 yes
O(6) Cl(2) O(6) 52(3) . . 8_545 yes
O(6) Cl(2) O(6) 77(5) . . 2_655 yes
O(6) Cl(2) O(7) 120(3) . . . yes
O(6) Cl(2) O(7) 95(6) . . 7_555 yes
O(6) Cl(2) O(7) 74(6) . . 8_545 yes
O(6) Cl(2) O(7) 47(3) . . 2_655 yes
O(6) Cl(2) O(6) 77(5) 7_555 . 8_545 yes
O(6) Cl(2) O(6) 52(3) 7_555 . 2_655 yes
O(6) Cl(2) O(7) 74(6) 7_555 . . yes
O(6) Cl(2) O(7) 120(3) 7_555 . 7_555 yes
O(6) Cl(2) O(7) 47(3) 7_555 . 8_545 yes
O(6) Cl(2) O(7) 95(6) 7_555 . 2_655 yes
O(6) Cl(2) O(6) 52(3) 8_545 . 2_655 yes
O(6) Cl(2) O(7) 95(6) 8_545 . . yes
O(6) Cl(2) O(7) 47(3) 8_545 . 7_555 yes
O(6) Cl(2) O(7) 120(3) 8_545 . 8_545 yes
O(6) Cl(2) O(7) 74(6) 8_545 . 2_655 yes
O(6) Cl(2) O(7) 47(3) 2_655 . . yes
O(6) Cl(2) O(7) 74(6) 2_655 . 7_555 yes
O(6) Cl(2) O(7) 95(6) 2_655 . 8_545 yes
O(6) Cl(2) O(7) 120(3) 2_655 . 2_655 yes
O(7) Cl(2) O(7) 89.3(3) . . 7_555 yes
O(7) Cl(2) O(7) 89.4(3) . . 8_545 yes
O(7) Cl(2) O(7) 167(3) . . 2_655 yes
O(7) Cl(2) O(7) 167(3) 7_555 . 8_545 yes
O(7) Cl(2) O(7) 89.4(3) 7_555 . 2_655 yes
O(7) Cl(2) O(7) 89.3(3) 8_545 . 2_655 yes
Gd O(1) C(1) 138.7(6) . . . yes
Gd O(2) C(4) 142(1) . . . yes
Gd O(2) C(8) 141(1) . . . yes
C(4) O(2) C(8) 39(1) . . . yes
Cl(2) O(6) O(6) 63(1) . . 7_555 yes
Cl(2) O(6) O(6) 63(1) . . 8_545 yes
Cl(2) O(6) O(6) 51(2) . . 2_655 yes
Cl(2) O(6) O(7) 58(4) . . 8_545 yes
Cl(2) O(6) O(7) 77(3) . . 2_655 yes
O(6) O(6) O(6) 89.98(1) 7_555 . 8_545 yes
O(6) O(6) O(6) 44.991(8) 7_555 . 2_655 yes
O(6) O(6) O(7) 41(7) 7_555 . 8_545 yes
O(6) O(6) O(7) 131(7) 7_555 . 2_655 yes
O(6) O(6) O(6) 44.991(8) 8_545 . 2_655 yes
O(6) O(6) O(7) 116(7) 8_545 . 8_545 yes
O(6) O(6) O(7) 97(11) 8_545 . 2_655 yes
O(6) O(6) O(7) 77(8) 2_655 . 8_545 yes
O(6) O(6) O(7) 124(6) 2_655 . 2_655 yes
O(7) O(6) O(7) 94(6) 8_545 . 2_655 yes
Cl(2) O(7) O(6) 46(2) . . 7_555 yes
Cl(2) O(7) O(6) 55(2) . . 2_655 yes
O(6) O(7) O(6) 41(5) 7_555 . 2_655 yes
C(1) N(1) C(2) 120.3(9) . . . yes
C(1) N(1) C(3) 121.2(10) . . . yes
C(2) N(1) C(3) 118.5(9) . . . yes
N(3) N(2) C(4) 46(1) . . . yes
N(3) N(2) C(6) 71(2) . . . yes
N(3) N(2) C(7) 155(2) . . . yes
N(3) N(2) C(8) 87(2) . . . yes
C(4) N(2) C(6) 117(2) . . . yes
C(4) N(2) C(7) 110(1) . . . yes
C(4) N(2) C(8) 40(2) . . . yes
C(6) N(2) C(7) 129(1) . . . yes
C(6) N(2) C(8) 158(3) . . . yes
C(7) N(2) C(8) 70(2) . . . yes
N(2) N(3) C(4) 90(2) . . . yes
N(2) N(3) C(5) 163(2) . . . yes
N(2) N(3) C(6) 72(2) . . . yes
N(2) N(3) C(8) 49(2) . . . yes
C(4) N(3) C(5) 73(2) . . . yes
C(4) N(3) C(6) 162(3) . . . yes
C(4) N(3) C(8) 41(2) . . . yes
C(5) N(3) C(6) 123(1) . . . yes
C(5) N(3) C(8) 115(2) . . . yes
C(6) N(3) C(8) 121(3) . . . yes
O(1) C(1) N(1) 123.7(8) . . . yes
O(2) C(4) N(2) 121(2) . . . yes
O(2) C(4) N(3) 164(3) . . . yes
O(2) C(4) C(5) 124(2) . . . yes
O(2) C(4) C(8) 73(3) . . . yes
N(2) C(4) N(3) 42(1) . . . yes
N(2) C(4) C(5) 113(2) . . . yes
N(2) C(4) C(8) 48(3) . . . yes
N(3) C(4) C(5) 71(2) . . . yes
N(3) C(4) C(8) 91(4) . . . yes
C(5) C(4) C(8) 162(4) . . . yes
N(3) C(5) C(4) 35(1) . . . yes
N(2) C(6) N(3) 35.7(9) . . . yes
N(2) C(7) C(8) 39(1) . . . yes
O(2) C(8) N(2) 157(4) . . . yes
O(2) C(8) N(3) 114(3) . . . yes
O(2) C(8) C(4) 66(3) . . . yes
O(2) C(8) C(7) 131(2) . . . yes
N(2) C(8) N(3) 43(1) . . . yes
N(2) C(8) C(4) 90(4) . . . yes
N(2) C(8) C(7) 70(2) . . . yes
N(3) C(8) C(4) 47(2) . . . yes
N(3) C(8) C(7) 113(3) . . . yes
C(4) C(8) C(7) 159(4) . . . yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd O(1) 2.409(7) . . yes
Gd O(1) 2.408(7) . 2_555 yes
Gd O(1) 2.408(7) . 5_555 yes
Gd O(1) 2.408(7) . 6_555 yes
Gd O(2) 2.355(6) . . yes
Gd O(2) 2.355(7) . 2_555 yes
Gd O(2) 2.355(6) . 5_555 yes
Gd O(2) 2.355(6) . 6_555 yes
Cl(1) O(3) 1.35(1) . . yes
Cl(1) O(3) 1.35(1) . 5_556 yes
Cl(1) O(4) 1.38(1) . . yes
Cl(1) O(4) 1.38(1) . 5_556 yes
Cl(2) O(5) 1.38(2) . . yes
Cl(2) O(6) 1.21(4) . . yes
Cl(2) O(6) 1.21(4) . 7_555 yes
Cl(2) O(6) 1.21(4) . 8_545 yes
Cl(2) O(6) 1.21(4) . 2_655 yes
Cl(2) O(7) 1.44(3) . . yes
Cl(2) O(7) 1.44(3) . 7_555 yes
Cl(2) O(7) 1.44(3) . 8_545 yes
Cl(2) O(7) 1.44(3) . 2_655 yes
O(1) C(1) 1.24(1) . . yes
O(2) C(4) 1.24(3) . . yes
O(2) C(8) 1.30(4) . . yes
O(6) O(6) 1.08(7) . 7_555 yes
O(6) O(6) 1.08(7) . 8_545 yes
O(6) O(6) 1.5(1) . 2_655 yes
O(6) O(7) 1.6(1) . 8_545 yes
O(6) O(7) 1.08(7) . 2_655 yes
N(1) C(1) 1.32(1) . . yes
N(1) C(2) 1.46(2) . . yes
N(1) C(3) 1.45(1) . . yes
N(2) N(3) 0.90(2) . . yes
N(2) C(4) 1.33(3) . . yes
N(2) C(6) 1.48(2) . . yes
N(2) C(7) 1.48(2) . . yes
N(2) C(8) 0.99(3) . . yes
N(3) C(4) 0.97(3) . . yes
N(3) C(5) 1.58(3) . . yes
N(3) C(6) 1.46(3) . . yes
N(3) C(8) 1.31(4) . . yes
C(4) C(5) 1.60(3) . . yes
C(4) C(8) 0.87(4) . . yes
C(7) C(8) 1.47(4) . . yes
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
O(2) O(4) 3.59(1) . 5_556 ?
O(3) C(6) 3.40(3) . . ?
O(3) C(6) 3.58(2) . 7_555 ?
O(4) C(4) 3.40(3) . 5_556 ?
O(4) C(8) 3.42(3) . 5_556 ?
O(4) C(3) 3.50(2) . 1_556 ?
O(4) N(3) 3.51(2) . 5_556 ?
O(4) C(1) 3.54(1) . 1_556 ?
O(4) N(2) 3.56(2) . 5_556 ?
O(5) C(6) 3.59(2) . 8_545 ?
O(5) C(6) 3.59(2) . 2_655 ?
O(5) C(6) 3.59(2) . 7_555 ?
O(5) C(6) 3.59(2) . . ?
O(6) C(3) 3.22(6) . . ?
O(6) N(1) 3.46(7) . . ?
O(7) C(2) 3.21(4) . 2_655 ?
O(7) N(1) 3.26(3) . 2_655 ?
O(7) C(5) 3.29(6) . 2_655 ?
O(7) C(3) 3.49(4) . 2_655 ?
C(7) C(7) 3.57(2) . 6_556 ?
loop_
_cod_changelog_entry_id
_cod_changelog_entry_author
_cod_changelog_entry_date
_cod_changelog_entry_text
1 'Vaitkus, Antanas' 2022-04-22T19:05:00+03:00
'Updated bibliographic information.'
