Synthesis and photoluminescence properties of polymer chains based on pre-designed heterometallic Al<sub>4</sub>Ln<sub>4</sub> molecular rings.
Sun, Qian-Ru; Luo, Dan; Lv, Yaokang; Fang, Wei-Hui; Zhang, Jian; Chemical communications (Cambridge, England) 60 (2024) 7574–7577; doi:10.1039/d4cc01611d

data_7133236
_publ_section_title
;
 Synthesis and photoluminescence properties of polymer chains based on
 pre-designed heterometallic Al<sub>4</sub>Ln<sub>4</sub> molecular rings.
;
_journal_issue                   59
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              7574
_journal_page_last               7577
_journal_paper_doi               10.1039/d4cc01611d
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         '0.5(C96 H192 Al8 Eu8 N16 O64)'
_chemical_formula_sum            'C48 H96 Al4 Eu4 N8 O32'
_chemical_formula_weight         2013.08
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2024-06-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-06-04 deposited with the CCDC.	2024-06-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 117.950(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.7753(5)
_cell_length_b                   10.2408(2)
_cell_length_c                   29.8910(6)
_cell_measurement_reflns_used    17424
_cell_measurement_temperature    99.99(13)
_cell_measurement_theta_max      60.3330
_cell_measurement_theta_min      2.8960
_cell_volume                     7510.5(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(13)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.954
_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     27.00 105.00   0.50    2.20    --   72.28-117.00  90.00  156
  2  \w     92.00 118.00   0.50    2.20    --   72.28 117.00 178.00   52
  3  \w     75.00 100.00   0.50    2.20    --   72.28 162.00 -31.00   50
  4  \w     56.00 144.00   0.50    2.20    --   72.28  57.00-180.00  176
  5  \w   -140.00-115.00   0.50    2.20    --  -74.78-117.00  90.00   50
  6  \w   -148.00-103.00   0.50    2.20    --  -74.78 -99.00 150.00   90
  7  \w   -148.00 -88.00   0.50    2.20    --  -74.78 -99.00 -60.00  120
  8  \w    -74.00 -39.00   0.50    0.55    --   -1.25 -57.00-120.00   70
  9  \w    -19.00  14.00   0.50    0.55    --   -1.25 -57.00-120.00   66
 10  \w    -89.00 -64.00   0.50    2.20    --  -74.78 -57.00 150.00   50
 11  \w   -148.00-122.00   0.50    2.20    --  -74.78 -57.00 150.00   52
 12  \w   -107.00 -19.00   0.50    2.20    --  -74.78 117.00 178.00  176
 13  \w   -111.00 -86.00   0.50    2.20    --  -74.78 162.00 -31.00   50
 14  \w    -91.00  -2.00   0.50    2.20    --  -74.78  57.00-180.00  178
 15  \w    -71.00  -9.00   0.50    2.20    --  -74.78  38.00-180.00  124
 16  \w    -70.00 -45.00   0.50    2.20    --  -74.78  38.00 150.00   50
 17  \w     -3.00  31.00   0.50    0.55    --   -1.25  38.00 120.00   68
 18  \w     43.00  69.00   0.50    0.55    --   -1.25  38.00 120.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0301049000
_diffrn_orient_matrix_UB_12      0.0902823000
_diffrn_orient_matrix_UB_13      0.0340743000
_diffrn_orient_matrix_UB_21      0.0352116000
_diffrn_orient_matrix_UB_22      -0.0927275000
_diffrn_orient_matrix_UB_23      0.0280849000
_diffrn_orient_matrix_UB_31      0.0288681000
_diffrn_orient_matrix_UB_32      0.0189743000
_diffrn_orient_matrix_UB_33      -0.0248983000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.0517
_diffrn_reflns_av_unetI/netI     0.0397
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            29888
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         60.536
_diffrn_reflns_theta_min         2.910
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    17.957
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64697
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic light colourless'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.780
_exptl_crystal_description       block
_exptl_crystal_F_000             4000
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.960
_refine_diff_density_min         -0.990
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         8237
_refine_ls_number_restraints     80
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0473
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0538P)^2^+60.6526P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1077
_refine_ls_wR_factor_ref         0.1130
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6943
_reflns_number_total             8237
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc01611d2.cif
_cod_data_source_block           AlOC-195-Eu
_cod_depositor_comments
'Adding full bibliography for 7133236--7133243.cif.'
_cod_database_code               7133236
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Al Eu C N O'
_shelx_estimated_absorpt_t_max   0.412
_shelx_estimated_absorpt_t_min   0.267
_diffrn_oxdiff_digest_frames
;
017397ec40f7956690a1bac5a54e700f2e01630544e
;
_diffrn_oxdiff_digest_hkl
;
01f898a99324b2780c882124ac66e5a3d9259c
;
_reflns_odcompleteness_completeness 99.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     56.82
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C016-C017
 1.37 with sigma of 0.01
 C01A-N00N
 1.4 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C019) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C00Z) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C018) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C01B) \\sim Ueq, Uanis(C018) \\sim Ueq, Uanis(C016) \\sim Ueq,
Uanis(C017) \\sim Ueq, Uanis(C013) \\sim Ueq, Uanis(C01A) \\sim Ueq,
Uanis(C015) \\sim Ueq, Uanis(C014) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C01A) \\sim Ueq, Uanis(C6) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C7) \\sim Ueq, Uanis(C013) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Fixed Sof: C013(0.8) H01G(0.8) H01H(0.8) H01I(0.8) C01A(0.8) H01U(0.8)
 H01V(0.8) C2(0.5) H2A(0.5) H2B(0.5) C5(0.5) H5A(0.5) H5B(0.5) C6(0.2) H6A(0.2)
 H6B(0.2) C7(0.2) H7A(0.2) H7B(0.2) H7C(0.2)
5.a Riding coordinates:
 C013(H01G,H01H,H01I), C016(H01L,H01M), C017(H01N,H01O), C01A(H01U,H01V),
 C2(H2A,H2B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B,H7C)
5.b Secondary CH2 refined with riding coordinates:
 C00P(H00A,H00B), C00R(H00C,H00D), C00T(H00H,H00I), C00X(H00M,H00N), C00Y(H00O,
 H00P), C00Z(H00R,H00S), C010(H01A,H01B), C011(H01C,H01D), C012(H01E,H01F),
 C015(H01J,H01K), C018(H01P,H01Q), C01B(H01W,H01X)
5.c Aromatic/amide H refined with riding coordinates:
 C00Q(H00Q), C00U(H00U), C00V(H00V), C014(H014)
5.d Idealised Me refined as rotating group:
 C00S(H00E,H00F,H00G), C00W(H00J,H00K,H00L), C019(H01R,H01S,H01T)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              1058
_shelx_hkl_checksum              64344
_shelx_fab_checksum              75985
_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 2.375
_oxdiff_exptl_absorpt_empirical_full_min 0.308