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_7133240
_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 Dy8 N16 O64), C3 H7 N O'
_chemical_formula_sum            'C51 H103 Al4 Dy4 N9 O33'
_chemical_formula_weight         2128.34
_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   geom
_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                 98.946(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.1901(9)
_cell_length_b                   10.2991(3)
_cell_length_c                   27.6382(6)
_cell_measurement_reflns_used    9314
_cell_measurement_temperature    262(2)
_cell_measurement_theta_max      55.5770
_cell_measurement_theta_min      2.6880
_cell_volume                     8207.8(4)
_computing_cell_refinement       'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      262(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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     -7.00  28.00   0.50    0.17    --   -1.17 -99.00  90.00   70
  2  \w     -8.00  28.00   0.50    0.17    --   -1.17 -99.00  30.00   72
  3  \w     -5.00  21.00   0.50    0.17    --   -1.17 -99.00 -60.00   52
  4  \w     92.00 117.00   0.50    0.68    --   67.97 104.00 -57.00   50
  5  \w     88.00 139.00   0.50    0.68    --   67.97 125.00-120.00  102
  6  \w     53.00 128.00   0.50    0.68    --   67.97  57.00 -60.00  150
  7  \w     45.00 139.00   0.50    0.68    --   67.97  57.00 -90.00  188
  8  \w     32.00  86.00   0.50    0.68    --   67.97-104.00-159.00  108
  9  \w      3.00  45.00   0.50    0.68    --   67.97 -38.00 120.00   84
 10  \w     47.00  73.00   0.50    0.17    --   -1.17  57.00-150.00   52
 11  \w    -21.00  15.00   0.50    0.17    --   -1.17  57.00-150.00   72
 12  \w   -103.00 -13.00   0.50    0.68    --  -70.31 104.00 -57.00  180
 13  \w    -70.00 -23.00   0.50    0.68    --  -70.31  38.00-120.00   94
 14  \w   -119.00 -92.00   0.50    0.68    --  -70.31-104.00-159.00   54
 15  \w   -126.00-100.00   0.50    0.68    --  -70.31 -99.00 -90.00   52
 16  \w   -143.00-105.00   0.50    0.68    --  -70.31 -99.00  60.00   76
 17  \w   -146.00 -88.00   0.50    0.68    --  -70.31 -99.00  90.00  116
;
_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      -0.0277702000
_diffrn_orient_matrix_UB_12      0.0389150000
_diffrn_orient_matrix_UB_13      0.0314870000
_diffrn_orient_matrix_UB_21      0.0186944000
_diffrn_orient_matrix_UB_22      0.1188646000
_diffrn_orient_matrix_UB_23      0.0009801000
_diffrn_orient_matrix_UB_31      -0.0322030000
_diffrn_orient_matrix_UB_32      0.0355451000
_diffrn_orient_matrix_UB_33      -0.0375921000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.1070
_diffrn_reflns_av_unetI/netI     0.0886
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            22955
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        52.923
_diffrn_reflns_theta_max         52.923
_diffrn_reflns_theta_min         2.665
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    19.588
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.23553
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.85a (Rigaku Oxford Diffraction, 2023)
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    1.722
_exptl_crystal_description       block
_exptl_crystal_F_000             4208
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.053
_refine_diff_density_min         -1.282
_refine_diff_density_rms         0.202
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.933
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     484
_refine_ls_number_reflns         7185
_refine_ls_number_restraints     98
_refine_ls_restrained_S_all      0.931
_refine_ls_R_factor_all          0.0912
_refine_ls_R_factor_gt           0.0676
_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^)+(0.1421P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1759
_refine_ls_wR_factor_ref         0.1919
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5323
_reflns_number_total             7185
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc01611d2.cif
_cod_data_source_block           AlOC-195-Dy
_cod_depositor_comments
'Adding full bibliography for 7133236--7133243.cif.'
_cod_database_code               7133240
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Al Dy C H O N'
_shelx_estimated_absorpt_t_max   0.441
_shelx_estimated_absorpt_t_min   0.245
_reflns_odcompleteness_completeness 99.12
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     53.78
_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
 C2-O2
 1.4 with sigma of 0.01
3. Restrained planarity
 C2, N1, C3, C10
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(O007) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C10) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(N1) \\sim Ueq: with sigma of
0.1 and sigma for terminal atoms of 0.2
Uanis(N1) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C3) \\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(C017) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 O00B, O00D, N00O, C00Z, H00T, H00U, C013, H01E, C019, H01M, H01N, C01B, H01R,
 H01S, C01D, H01W, H01X, H01Y, N1, C3, H3A, H3B, H3C, C10, H10A, H10B, H10C, C2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Fixed Sof: N1(0.5) C3(0.5) H3A(0.5) H3B(0.5) H3C(0.5) C10(0.5) H10A(0.5)
 H10B(0.5) H10C(0.5) C2(0.5) H2(0.5) O2(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C00P(H00A,H00B), C00R(H00C,H00D), C00T(H00E,H00F), C00U(H00G,H00H), C00V(H00I,
 H00J), C00X(H00N,H00O), C00Y(H00P,H00R), C00Z(H00T,H00U), C011(H01A,H01B),
 C012(H01C,H01D), C013(H01E,H01F), C015(H01G,H01H), C016(H01I,H01J), C017(H01K,
 H01L), C019(H01M,H01N), C01B(H01R,H01S)
7.b Aromatic/amide H refined with riding coordinates:
 C00Q(H00Q), C00S(H00S), C010(H010), C014(H014), C2(H2)
7.c Idealised Me refined as rotating group:
 C00W(H00K,H00L,H00M), C01A(H01O,H01P,H01Q), C01C(H01T,H01U,H01V), C01D(H01W,
 H01X,H01Y), C3(H3A,H3B,H3C), C10(H10A,H10B,H10C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              57720
_shelx_hkl_checksum              64282
_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 5.116
_oxdiff_exptl_absorpt_empirical_full_min 0.138