Synthesis, crystal structure, and luminescence properties of a three-dimensional coordination polymer from europium(iii) carbonate hemioxalate hydrate
Takano, Rina; Ishida, Takayuki; Ay, Burak; CrystEngComm  (2022) –; doi:10.1039/D2CE01105K

data_7245721
_publ_section_title
;
 Synthesis, crystal structure, and luminescence properties of a
 three-dimensional coordination polymer from europium(iii) carbonate
 hemioxalate hydrate
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE01105K
_journal_year                    2022
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C2 H2 Eu O6'
_chemical_formula_sum            'C2 H2 Eu O6'
_chemical_formula_weight         273.999
_chemical_name_common            '[Eu(ox)0.5(CO3)(H2O)]'
_chemical_name_systematic        'Europium(III) Carbonate Hemioxalate Hydrate'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           38
_space_group_name_Hall           'A 2 -2'
_space_group_name_H-M_alt        'A m m 2'
_symmetry_Int_Tables_number      38
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2c77b6
_audit_creation_date             2022-05-13
_audit_creation_method
;
Olex2 1.5-ac5-018
(compiled 2021.09.08 svn.r13c46975 for Rigaku Oxford Diffraction, GUI svn.r6396)
;
_audit_update_record
;
2022-06-24 deposited with the CCDC.	2022-09-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   4.8070(4)
_cell_length_b                   15.1947(9)
_cell_length_c                   7.8938(6)
_cell_measurement_reflns_used    1334
_cell_measurement_temperature    100.8(4)
_cell_measurement_theta_max      31.7660
_cell_measurement_theta_min      4.2450
_cell_volume                     576.57(7)
_computing_cell_refinement       'CrysAlisPro 1.171.42.35a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.42.35a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.42.35a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5-ac5-018 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-018 (Dolomanov et al., 2009)'
_computing_structure_refinement
'olex2.refine 1.5-ac5-018 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.8(4)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.9848
_diffrn_measured_fraction_theta_max 0.8317
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     -3.00  24.00   0.50    0.20    --   -4.52  91.00 -47.00   54
  2  \w    -17.00  29.00   0.50    0.20    --    3.74 -99.00   0.00   92
  3  \w    -39.00  13.00   0.50    0.20    --   -4.52 -77.00 150.00  104
  4  \w    -75.00 -41.00   0.50    0.20    --   -4.52 -77.00 150.00   68
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0043292000
_diffrn_orient_matrix_UB_12      0.0452894000
_diffrn_orient_matrix_UB_13      0.0347467000
_diffrn_orient_matrix_UB_21      -0.0362123000
_diffrn_orient_matrix_UB_22      -0.0109173000
_diffrn_orient_matrix_UB_23      0.1307888000
_diffrn_orient_matrix_UB_31      0.0820494000
_diffrn_orient_matrix_UB_32      -0.0024137000
_diffrn_orient_matrix_UB_33      0.0593406000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0230
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_Laue_measured_fraction_full 0.9848
_diffrn_reflns_Laue_measured_fraction_max 0.8317
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            1613
_diffrn_reflns_point_group_measured_fraction_full 0.8728
_diffrn_reflns_point_group_measured_fraction_max 0.6918
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         31.84
_diffrn_reflns_theta_min         4.78
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    10.836
_exptl_absorpt_correction_T_max  0.476
_exptl_absorpt_correction_T_min  0.318
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.35a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.156
_exptl_crystal_description       prism
_exptl_crystal_F_000             500.597
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.8867
_refine_diff_density_min         -1.2569
_refine_diff_density_rms         0.1698
_refine_ls_abs_structure_details
'Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668.'
_refine_ls_abs_structure_Flack   0.3(2)
_refine_ls_d_res_high            0.6736
_refine_ls_d_res_low             4.2629
_refine_ls_goodness_of_fit_ref   1.0629
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    4
_refine_ls_number_parameters     59
_refine_ls_number_reflns         779
_refine_ls_number_restraints     64
_refine_ls_restrained_S_all      1.0193
_refine_ls_R_factor_all          0.0224
_refine_ls_R_factor_gt           0.0213
_refine_ls_shift/su_max          0.0010
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0303P)^2^+3.1050P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0519
_refine_ls_wR_factor_ref         0.0527
_reflns_Friedel_coverage         0.532
_reflns_limit_h_max              6
_reflns_limit_h_min              -6
_reflns_limit_k_max              20
_reflns_limit_k_min              -22
_reflns_limit_l_max              9
_reflns_limit_l_min              -10
_reflns_number_gt                755
_reflns_number_total             779
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2ce01105k2.cif
_cod_data_source_block           Eu_Burak4
_cod_original_sg_symbol_Hall     ' A 2 -2'
_cod_database_code               7245721
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C2H2Eu1O6
_chemical_oxdiff_usercomment     unclear
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.58(6)
 0.42(6)
2. Fixed Uiso
 At 1.5 times of:
  All O(H,H) groups
3. Restrained distances
 O5-H5b = O5-H5a
 0.84 with sigma of 0.005
 H5b-H5a
 1.33 with sigma of 0.005
4. Uiso/Uaniso restraints and constraints
O1 \\sim O2 \\sim C1 \\sim C2: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
O3 \\sim O4 \\sim C3: within 2A with sigma of 0.04 and sigma for terminal atoms
of 0.08 within 2A
Uanis(O5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 O1, O2, C1, C2
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O3, O4, C3
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
6.a Idealised tetrahedral OH refined as rotating group:
 O5(H5a), O5(H5b)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.923
_oxdiff_exptl_absorpt_empirical_full_min 0.400