Dysprosium complexes with mono-/di-carboxylate ligands—From simple dimers to 2D and 3D frameworks
Zhang, Yingjie; Bhadbhade, Mohan; Scales, Nicholas; Karatchevtseva, Inna; Price, Jason R.; Lu, Kim; Lumpkin, Gregory R.; Journal of Solid State Chemistry 219 (2014) 1–8; doi:10.1016/j.jssc.2014.07.007

data_1562211
_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 <i>et al</i>., 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+0.001xFc^2^\l^3^/sin(2\q)]^-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/[\s^2^(Fo^2^)+(0.0250P)^2^+0.6628P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(I)'
_cod_data_source_file            mmc2.cif
_cod_data_source_block           R3m
_cod_original_cell_volume        369.04(13)
_cod_database_code               1562211
_shelx_estimated_absorpt_t_min   0.888
_shelx_estimated_absorpt_t_max   0.901
_shelxl_version_number           2013-3
_shelx_res_checksum              62863
_shelx_hkl_checksum              99769