Structural, optical and phonon properties of formate-based MOF phosphors with ethylammonium cation
Ptak, Maciej; Pasińska, Katarzyna; Głuchowski, Paweł; Lukowiak, Anna; Ciupa, Aneta; Phys. Chem. Chem. Phys.  (2017) –; doi:10.1039/C7CP04005A

data_7228904
_publ_section_title
;
 Structural, optical and phonon properties of formate-based MOF phosphors
 with ethylammonium cation
;
_journal_name_full               'Phys. Chem. Chem. Phys.'
_journal_paper_doi               10.1039/C7CP04005A
_journal_year                    2017
_chemical_formula_moiety         'C4 H4 Er0.02 O8 Y0.91 Yb0.07, C2 H8 N'
_chemical_formula_sum            'C6 H12 Er0.02 N O8 Y0.91 Yb0.07'
_chemical_formula_weight         322.53
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-05-10
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2017-06-14 deposited with the CCDC.
2017-08-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.42(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.657(3)
_cell_length_b                   8.652(3)
_cell_length_c                   9.708(3)
_cell_measurement_reflns_used    7001
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.1180
_cell_measurement_theta_min      3.1470
_cell_volume                     546.1(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6249
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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     32.00 102.00   1.00    1.09    --   12.43-178.00 -90.00   70
  2  \w    -69.00  47.00   1.00    1.09    --   12.43 -77.00   0.00  116
  3  \w    -22.00  94.00   1.00    1.09    --   12.43  77.00  90.00  116
  4  \w   -103.00 -32.00   1.00    1.09    --  -13.52 178.00 150.00   71
  5  \w    -16.00  90.00   1.00    1.09    --   12.43  37.00 -30.00  106
  6  \w    -77.00 -32.00   1.00    1.09    --   12.43 178.00-180.00   45
  7  \w    -64.00  44.00   1.00    1.09    --   12.43 -57.00-180.00  108
  8  \w     35.00 104.00   1.00    1.09    --   12.43 178.00-180.00   69
  9  \w    -64.00  13.00   1.00    1.09    --   12.43 -57.00  30.00   77
 10  \w    -25.00  29.00   1.00    1.09    --  -13.52 -99.00 150.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0293640000
_diffrn_orient_matrix_UB_12      0.0752830000
_diffrn_orient_matrix_UB_13      -0.0168959000
_diffrn_orient_matrix_UB_21      0.0189118000
_diffrn_orient_matrix_UB_22      0.0205445000
_diffrn_orient_matrix_UB_23      0.0723713000
_diffrn_orient_matrix_UB_31      0.1033541000
_diffrn_orient_matrix_UB_32      -0.0251528000
_diffrn_orient_matrix_UB_33      0.0085288000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0398
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            10884
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.955
_diffrn_reflns_theta_min         3.188
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.640
_exptl_absorpt_correction_T_max  0.449
_exptl_absorpt_correction_T_min  0.288
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.962
_exptl_crystal_description       block
_exptl_crystal_F_000             322
_exptl_crystal_size_max          0.315
_exptl_crystal_size_mid          0.254
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.340
_refine_diff_density_min         -0.294
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details
;
 Flack x determined using 900 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.048(5)
_refine_ls_extinction_coef       0.040(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         2127
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0240
_refine_ls_R_factor_gt           0.0218
_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^)+(0.0203P)^2^+0.3597P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0493
_refine_ls_wR_factor_ref         0.0502
_reflns_Friedel_coverage         0.869
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                2038
_reflns_number_total             2127
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cp04005a2.cif
_cod_data_source_block           EtAYYbEr_293K
_cod_database_code               7228904
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C6 H12 N1 O8 Y0.95 Yb0.04 Er0.01'
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H) groups, All N(H,H,H) groups
2. Shared sites
{Y1, Yb1, Er1}
3. Uiso/Uaniso restraints and constraints
Uanis(Y1) = Uanis(Yb1) = Uanis(Er1)
4. Others
 Fixed Sof: Y1(0.91) Yb1(0.07) Er1(0.02)
5.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4)
5.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), N1(H1A,H1B,H1C)
;
_shelx_res_checksum              74326
_olex2_date_sample_data_collection 2017-01-17
_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 1.089
_oxdiff_exptl_absorpt_empirical_full_min 0.901