#------------------------------------------------------------------------------
#$Date: 2021-04-28 12:37:22 +0300 (Wed, 28 Apr 2021) $
#$Revision: 264638 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/22/1562211.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_1562211
loop_
_publ_author_name
'Zhang, Yingjie'
'Bhadbhade, Mohan'
'Scales, Nicholas'
'Karatchevtseva, Inna'
'Price, Jason R.'
'Lu, Kim'
'Lumpkin, Gregory R.'
_publ_section_title
;
 Dysprosium complexes with mono-/di-carboxylate ligands---From simple
 dimers to 2D and 3D frameworks
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              1
_journal_page_last               8
_journal_paper_doi               10.1016/j.jssc.2014.07.007
_journal_volume                  219
_journal_year                    2014
_chemical_formula_sum            'C3 H3 Dy O6'
_chemical_formula_weight         297.55
_space_group_crystal_system      trigonal
_space_group_IT_number           160
_space_group_name_Hall           'R 3 -2"'
_space_group_name_H-M_alt        'R 3 m :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   10.3840(15)
_cell_length_b                   10.3840(15)
_cell_length_c                   3.9520(8)
_cell_measurement_reflns_used    9980
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      2.5
_cell_volume                     369.04(11)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BLU-ICE (McPhillips et al., 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008) and OLEX-2 (Dolomanov et al., 2009)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_type            'ADSC Quantum 210r'
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  '3-BM1 Australian Synchrotron'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  Si<111>
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71080
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_unetI/netI     0.0141
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            1764
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.244
_diffrn_reflns_theta_max         26.355
_diffrn_reflns_theta_min         3.925
_diffrn_source                   'Synchrotron BM'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    15.146
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    4.017
_exptl_crystal_description       tetrahedra
_exptl_crystal_F_000             405
_exptl_crystal_size_max          0.008
_exptl_crystal_size_mid          0.007
_exptl_crystal_size_min          0.007
_refine_diff_density_max         0.306
_refine_diff_density_min         -0.641
_refine_diff_density_rms         0.107
_refine_ls_abs_structure_details
;
 Flack x determined using 93 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.075(19)
_refine_ls_extinction_coef       0.0065(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.831
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     23
_refine_ls_number_reflns         192
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.828
_refine_ls_R_factor_all          0.0091
_refine_ls_R_factor_gt           0.0091
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0250P)²+0.6628P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0231
_refine_ls_wR_factor_ref         0.0231
_reflns_Friedel_coverage         0.939
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                192
_reflns_number_total             192
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            mmc2.cif
_cod_data_source_block           R3m
_cod_original_cell_volume        369.04(13)
_cod_database_code               1562211
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.888
_shelx_estimated_absorpt_t_max   0.901
_shelxl_version_number           2013-3
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'-y+2/3, -x+1/3, z+1/3'
'-x+y+2/3, y+1/3, z+1/3'
'x+2/3, x-y+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-y+1/3, -x+2/3, z+2/3'
'-x+y+1/3, y+2/3, z+2/3'
'x+1/3, x-y+2/3, z+2/3'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.0000 0.0000 0.06803(2) 0.0031(3) Uani 1 6 d S T P . .
O1 O 0.1322(3) 0.2645(7) 0.0495(13) 0.0102(12) Uani 1 2 d S T P . .
O2 O 0.2496(3) 0.4993(6) 0.2295(13) 0.0081(11) Uani 1 2 d S T P . .
C1 C 0.1795(5) 0.3589(10) 0.278(2) 0.0096(14) Uani 1 2 d S T P . .
H1CA H 0.1626 0.3251 0.5002 0.012 Uiso 1 2 calc R U 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'
Dy Dy -0.1892 4.4098 '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
O1 Dy1 O1 119.906(14) . 2
O1 Dy1 O1 119.906(14) . 3
O1 Dy1 O1 119.906(14) 2 3
O1 Dy1 O2 73.71(12) . 8
O1 Dy1 O2 129.35(18) 2 8
O1 Dy1 O2 73.71(12) 3 8
O1 Dy1 O2 129.35(18) . 7_445
O1 Dy1 O2 73.71(12) 2 7_445
O1 Dy1 O2 73.71(12) 3 7_445
O2 Dy1 O2 63.8(2) 8 7_445
O1 Dy1 O2 73.71(12) . 9_455
O1 Dy1 O2 73.71(12) 2 9_455
O1 Dy1 O2 129.36(18) 3 9_455
O2 Dy1 O2 63.8(2) 8 9_455
O2 Dy1 O2 63.8(2) 7_445 9_455
O1 Dy1 O2 125.25(17) . 7_444
O1 Dy1 O2 71.01(12) 2 7_444
O1 Dy1 O2 71.01(12) 3 7_444
O2 Dy1 O2 144.72(9) 8 7_444
O2 Dy1 O2 105.4(2) 7_445 7_444
O2 Dy1 O2 144.72(9) 9_455 7_444
O1 Dy1 O2 71.01(12) . 8_554
O1 Dy1 O2 125.25(17) 2 8_554
O1 Dy1 O2 71.01(12) 3 8_554
O2 Dy1 O2 105.4(2) 8 8_554
O2 Dy1 O2 144.72(9) 7_445 8_554
O2 Dy1 O2 144.72(9) 9_455 8_554
O2 Dy1 O2 62.8(2) 7_444 8_554
O1 Dy1 O2 71.01(12) . 9_454
O1 Dy1 O2 71.01(12) 2 9_454
O1 Dy1 O2 125.25(17) 3 9_454
O2 Dy1 O2 144.72(9) 8 9_454
O2 Dy1 O2 144.72(9) 7_445 9_454
O2 Dy1 O2 105.4(2) 9_455 9_454
O2 Dy1 O2 62.8(2) 7_444 9_454
O2 Dy1 O2 62.8(2) 8_554 9_454
O1 Dy1 Dy1 88.23(13) . 1_554
O1 Dy1 Dy1 88.23(13) 2 1_554
O1 Dy1 Dy1 88.23(13) 3 1_554
O2 Dy1 Dy1 142.41(13) 8 1_554
O2 Dy1 Dy1 142.41(13) 7_445 1_554
O2 Dy1 Dy1 142.41(13) 9_455 1_554
O2 Dy1 Dy1 37.02(13) 7_444 1_554
O2 Dy1 Dy1 37.02(13) 8_554 1_554
O2 Dy1 Dy1 37.02(13) 9_454 1_554
O1 Dy1 Dy1 91.77(13) . 1_556
O1 Dy1 Dy1 91.77(13) 2 1_556
O1 Dy1 Dy1 91.77(13) 3 1_556
O2 Dy1 Dy1 37.59(13) 8 1_556
O2 Dy1 Dy1 37.59(13) 7_445 1_556
O2 Dy1 Dy1 37.59(13) 9_455 1_556
O2 Dy1 Dy1 142.98(13) 7_444 1_556
O2 Dy1 Dy1 142.98(13) 8_554 1_556
O2 Dy1 Dy1 142.98(13) 9_454 1_556
Dy1 Dy1 Dy1 180.0 1_554 1_556
C1 O1 Dy1 131.5(5) . .
C1 O2 Dy1 136.2(5) . 13_554
C1 O2 Dy1 118.4(5) . 13
Dy1 O2 Dy1 105.4(2) 13_554 13
O1 C1 O2 124.7(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Dy1 O1 2.379(6) .
Dy1 O1 2.380(6) 2
Dy1 O1 2.380(6) 3
Dy1 O2 2.468(5) 8
Dy1 O2 2.468(5) 7_445
Dy1 O2 2.468(5) 9_455
Dy1 O2 2.500(5) 7_444
Dy1 O2 2.500(5) 8_554
Dy1 O2 2.500(5) 9_454
Dy1 Dy1 3.9520(8) 1_554
Dy1 Dy1 3.9520(8) 1_556
O1 C1 1.239(10) .
O2 C1 1.276(11) .
O2 Dy1 2.468(5) 13_554
O2 Dy1 2.500(5) 13
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
Dy1 O1 C1 O2 180.000(2) . . . .
Dy1 O2 C1 O1 -0.001(4) 13_554 . . .
Dy1 O2 C1 O1 180.001(2) 13 . . .
