Solution-processable Yb/Er 2D-layered metallorganic frameworks with high NIR-emission quantum yields
Artizzu, Flavia; Atzori, Matteo; Liu, Jing; Mara, Dimitrije; Van Hecke, Kristof; Van Deun, Rik; Journal of Materials Chemistry C 7 (2019) 11207–; doi:10.1039/C9TC03698A

data_7237951
_publ_section_title
;
 Solution-processable Yb/Er 2D-layered metallorganic frameworks with high
 NIR-emission quantum yields
;
_journal_issue                   36
_journal_name_full               'Journal of Materials Chemistry C'
_journal_page_first              11207
_journal_paper_doi               10.1039/C9TC03698A
_journal_volume                  7
_journal_year                    2019
_chemical_formula_moiety         'C65.89 H72 Cl6.11 Er4 N5.89 O36 S12'
_chemical_formula_sum            'C65.89 H72 Cl6.11 Er4 N5.89 O36 S12'
_chemical_formula_weight         2792.81
_space_group_crystal_system      tetragonal
_space_group_IT_number           87
_space_group_name_Hall           '-I 4'
_space_group_name_H-M_alt        'I 4/m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-05-17
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-05-17 deposited with the CCDC.	2019-08-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   19.7597(10)
_cell_length_b                   19.7597(10)
_cell_length_c                   14.6295(10)
_cell_measurement_reflns_used    2987
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      69.2060
_cell_measurement_theta_min      3.7420
_cell_volume                     5712.0(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4839
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.955
_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    -83.00  38.00   1.00    7.00    --  -41.80  19.00  60.00  121
  2  \w     23.00  98.00   1.00    7.00    --   41.80-125.00 120.00   75
  3  \w    101.00 178.00   1.00  160.00    --  109.13 107.00 -98.00   77
  4  \w     94.00 178.00   1.00  160.00    --  109.13 125.00 -30.00   84
  5  \w     94.00 178.00   1.00  160.00    --  109.13 125.00-150.00   84
  6  \w     36.00  96.00   1.00  160.00    --  109.13-125.00 -90.00   60
  7  \w   -116.00 -17.00   1.00    7.00    --  -41.80 -38.00-120.00   99
  8  \w   -118.00  -9.00   1.00    7.00    --  -41.80 -77.00 120.00  109
  9  \w    -92.00 -59.00   1.00    7.00    --  -41.80 125.00-150.00   33
 10  \w   -118.00  -9.00   1.00    7.00    --  -41.80 -77.00  30.00  109
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0639670000
_diffrn_orient_matrix_UB_12      0.0052459000
_diffrn_orient_matrix_UB_13      -0.0598922000
_diffrn_orient_matrix_UB_21      0.0406930000
_diffrn_orient_matrix_UB_22      0.0250928000
_diffrn_orient_matrix_UB_23      0.0831790000
_diffrn_orient_matrix_UB_31      0.0183463000
_diffrn_orient_matrix_UB_32      -0.0735830000
_diffrn_orient_matrix_UB_33      0.0241855000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_unetI/netI     0.0165
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            13234
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.107
_diffrn_reflns_theta_min         3.759
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.192
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.696
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.623
_exptl_crystal_description       block
_exptl_crystal_F_000             2728.9
_exptl_crystal_size_max          0.231
_exptl_crystal_size_mid          0.219
_exptl_crystal_size_min          0.164
_refine_diff_density_max         0.599
_refine_diff_density_min         -0.558
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     171
_refine_ls_number_reflns         2937
_refine_ls_number_restraints     353
_refine_ls_restrained_S_all      1.318
_refine_ls_R_factor_all          0.1828
_refine_ls_R_factor_gt           0.1255
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+50.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1707
_refine_ls_wR_factor_ref         0.1909
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1154
_reflns_number_total             2937
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9tc03698a4.cif
_cod_data_source_block           er_cncl_3
_cod_original_cell_volume        5712.0(7)
_cod_database_code               7237951
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C65.89 H72 Cl6.11 Er4 N5.89 O36 S12'
_reflns_odcompleteness_completeness 98.65
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 S1-O5 = S2-O6
 1.515 with sigma of 0.01
 S1-C7 = S1-C8 = S2-C9 = S2-C10
 1.776 with sigma of 0.01
 C1-O1 = C3-O4 = C5-O2 = C4-O3
 1.256 with sigma of 0.01
 C1-C2 = C2-C3 = C5-C6
 1.398 with sigma of 0.01
 C4-C5
 1.53 with sigma of 0.01
 C6-Cl1B = C2-Cl1A
 1.73 with sigma of 0.01
 C6-C11A = C2-C11B
 1.43 with sigma of 0.01
 N1A-C11A = N1B-C11B
 1.134 with sigma of 0.01
 C7-O5 = C8-O5 = C9-O6 = C10-O6
 2.619 with sigma of 0.02
 C7-C8 = C9-C10
 2.688 with sigma of 0.02
 C1-Cl1A = C3-Cl1A
 2.7 with sigma of 0.02
 C1-C11B = C3-C11B
 2.45 with sigma of 0.02
 C5-Cl1B
 2.7 with sigma of 0.02
 C5-C11A
 2.45 with sigma of 0.02
 C2-N1B = C3-N1B = C5-N1A
 3.5 with sigma of 0.02
3. Restrained planarity
 C1, C2, C3, C11B, Cl1A, N1B
 with sigma of 0.01
 C4, C5, C6, C11A, Cl1B, N1A
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.02 and sigma
for terminal atoms of 0.04
Uanis(Cl1A) = Uanis(Cl1B) = Uanis(C11A) = Uanis(C11B) = Uanis(N1A) = Uanis(N1B)
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.0035 and sigma for 1-3 distances of 0.0035
6. Others
 Sof(C11B)=Sof(N1B)=1-FVAR(1)
 Sof(Cl1B)=0.5*(1-FVAR(2))
 Sof(C11A)=Sof(N1A)=0.5*FVAR(2)
 Sof(Cl1A)=FVAR(1)
 Fixed Sof: H7A(0.5) H7B(0.5) H7C(0.5) H8A(0.5) H8B(0.25) H8C(0.5) S1(0.5)
7.a Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C)
;
_shelx_res_checksum              39427
_shelx_fab_checksum              98507
_olex2_exptl_crystal_mounting_method 'mounted on a nylon loop'
_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
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 3.578
_oxdiff_exptl_absorpt_empirical_full_min 0.489