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_7133242
_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         'C48 H96 Al4 N8 O32 Tm4'
_chemical_formula_sum            'C48 H96 Al4 N8 O32 Tm4'
_chemical_formula_weight         2080.96
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2024-06-02
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2024-06-04 deposited with the CCDC.	2024-06-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.182(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.5990(6)
_cell_length_b                   10.1083(3)
_cell_length_c                   28.8433(8)
_cell_measurement_reflns_used    11450
_cell_measurement_temperature    100.00(13)
_cell_measurement_theta_max      59.8690
_cell_measurement_theta_min      2.7200
_cell_volume                     7943.6(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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(13)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.916
_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   -112.00 -16.00   0.50    0.36    --  -78.59  83.00  83.00  192
  2  \w     -6.00  20.00   0.50    0.09    --   -1.41  83.00  83.00   52
  3  \w    -19.00  61.00   0.50    0.09    --   -1.41  57.00-180.00  160
  4  \w    -48.00  -7.00   0.50    0.36    --  -78.59  57.00-150.00   82
  5  \w    -95.00 -55.00   0.50    0.36    --  -78.59  57.00-150.00   80
  6  \w   -153.00 -44.00   0.50    0.36    --  -78.59 -19.00 -30.00  218
  7  \w   -151.00 -89.00   0.50    0.36    --  -78.59 -99.00 120.00  124
  8  \w   -141.00-116.00   0.50    0.36    --  -78.59 -83.00 -36.00   50
  9  \w   -143.00 -56.00   0.50    0.36    --  -78.59 -57.00 -60.00  174
 10  \w    -13.00  13.00   0.50    0.09    --   -1.41 -83.00 -36.00   52
 11  \w     -8.00  29.00   0.50    0.09    --   -1.41 -99.00  60.00   74
 12  \w      2.00  70.00   0.50    0.36    --   75.78 -38.00 -30.00  136
 13  \w     46.00  72.00   0.50    0.36    --   75.78 -83.00 -36.00   52
 14  \w    114.00 140.00   0.50    0.36    --   75.78  83.00  83.00   52
 15  \w     82.00 143.00   0.50    0.36    --   75.78 125.00   0.00  122
 16  \w    -17.00  59.00   0.50    0.09    --   -1.41  57.00 -90.00  152
 17  \w     -8.00  17.00   0.50    0.09    --   -1.41 -99.00   0.00   50
 18  \w     75.00 102.00   0.50    0.36    --   75.78  77.00-150.00   54
 19  \w      6.00  31.50   0.50    0.36    --   75.78 -38.00 -60.00   51
;
_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      -0.0231053000
_diffrn_orient_matrix_UB_12      -0.1066037000
_diffrn_orient_matrix_UB_13      -0.0204277000
_diffrn_orient_matrix_UB_21      -0.0060096000
_diffrn_orient_matrix_UB_22      -0.0460568000
_diffrn_orient_matrix_UB_23      0.0421906000
_diffrn_orient_matrix_UB_31      -0.0429760000
_diffrn_orient_matrix_UB_32      0.0638854000
_diffrn_orient_matrix_UB_33      -0.0035389000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.0917
_diffrn_reflns_av_unetI/netI     0.0831
_diffrn_reflns_Laue_measured_fraction_full 0.960
_diffrn_reflns_Laue_measured_fraction_max 0.916
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            25357
_diffrn_reflns_point_group_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.916
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         60.340
_diffrn_reflns_theta_min         2.698
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    15.200
_exptl_absorpt_correction_T_max  0.484
_exptl_absorpt_correction_T_min  0.283
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.85a (Rigaku Oxford Diffraction, 2023)
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            'clear light white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.740
_exptl_crystal_description       block
_exptl_crystal_F_000             4096
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.624
_refine_diff_density_min         -1.305
_refine_diff_density_rms         0.254
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     437
_refine_ls_number_reflns         8304
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1188
_refine_ls_R_factor_gt           0.0884
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1032P)^2^+326.9733P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2004
_refine_ls_wR_factor_ref         0.2193
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6250
_reflns_number_total             8304
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc01611d2.cif
_cod_data_source_block           AlOC-195-Tm
_cod_depositor_comments
'Adding full bibliography for 7133236--7133243.cif.'
_cod_database_code               7133242
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         Al4Tm4H96C32N8
_shelx_estimated_absorpt_t_max   0.517
_shelx_estimated_absorpt_t_min   0.376
_reflns_odcompleteness_completeness 97.68
_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. Uiso/Uaniso restraints and constraints
Uanis(C00S) \\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(O006) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C00O) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O005) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C00O(H00A,H00B), C00Q(H00F,H00G), C00U(H00H,H00I), C00V(H00J,H00K), C00X(H00L,
 H00M), C00Z(H00N,H00O), C010(H01A,H01B), C011(H01C,H01D), C012(H01E,H01F),
 C014(H01J,H01K), C016(H01O,H01P), C017(H01Q,H01R), C018(H01S,H01T), C019(H01U,
 H01V), C01A(H01W,H01X), C01D(H01Z,HB)
3.b Aromatic/amide H refined with riding coordinates:
 C00S(H00S), C00T(H00T), C00W(H00W), C00Y(H00Y)
3.c Idealised Me refined as rotating group:
 C00P(H00C,H00D,H00E), C013(H01G,H01H,H01I), C015(H01L,H01M,H01N), C01B(H01Y,H,
 HA)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              57897
_shelx_hkl_checksum              65162
_shelx_fab_checksum              98227
_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 3.971
_oxdiff_exptl_absorpt_empirical_full_min 0.281