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_7133243
_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 Tb4, 2(C3 H7 N O)'
_chemical_formula_sum            'C54 H110 Al4 N10 O34 Tb4'
_chemical_formula_weight         2187.11
_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             2024-06-15
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2024-06-15 deposited with the CCDC.	2024-06-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.256(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.9239(5)
_cell_length_b                   10.1329(2)
_cell_length_c                   28.9993(5)
_cell_measurement_reflns_used    13298
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      53.5190
_cell_measurement_theta_min      2.7780
_cell_volume                     8098.5(3)
_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  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_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   -136.00-110.00   0.50    1.10    --  -65.64  11.00 -56.00   52
  2  \w    -91.00 -31.00   0.50    1.10    --  -65.64 125.00 -60.00  120
  3  \w    -89.00   3.00   0.50    1.10    --  -65.64  57.00  90.00  184
  4  \w     12.00  76.00   0.50    0.41    --   -1.17  11.00 -56.00  128
  5  \w    -13.00 146.00   0.50    1.10    --   63.30  11.00 -56.00  318
  6  \w     10.00  88.00   0.50    1.10    --   63.30 -77.00  30.00  156
  7  \w     70.00  96.00   0.50    1.10    --   63.30-125.00-150.00   52
  8  \w     -6.00  35.00   0.50    0.41    --   -1.17 -99.00-180.00   82
  9  \w   -137.00-105.00   0.50    1.10    --  -65.64-125.00-150.00   64
 10  \w   -135.00-110.00   0.50    1.10    --  -65.64-125.00 -60.00   50
 11  \w   -138.00-108.00   0.50    1.10    --  -65.64-125.00 -30.00   60
 12  \w    -78.00 -14.00   0.50    0.41    --   -1.17 -11.00 130.00  128
 13  \w   -105.00   8.00   0.50    1.10    --  -65.64 -11.00 130.00  226
;
_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      -0.0101040000
_diffrn_orient_matrix_UB_12      0.0156795000
_diffrn_orient_matrix_UB_13      0.0432879000
_diffrn_orient_matrix_UB_21      0.0474343000
_diffrn_orient_matrix_UB_22      0.0114156000
_diffrn_orient_matrix_UB_23      0.0165404000
_diffrn_orient_matrix_UB_31      -0.0029262000
_diffrn_orient_matrix_UB_32      0.1306929000
_diffrn_orient_matrix_UB_33      -0.0066165000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.0622
_diffrn_reflns_av_unetI/netI     0.0517
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            25133
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        52.930
_diffrn_reflns_theta_max         52.930
_diffrn_reflns_theta_min         2.788
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    18.998
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48077
_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            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.794
_exptl_crystal_description       block
_exptl_crystal_F_000             4352
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.666
_refine_diff_density_min         -1.979
_refine_diff_density_rms         0.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     493
_refine_ls_number_reflns         6910
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0549
_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^)+(0.1010P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1366
_refine_ls_wR_factor_ref         0.1424
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5721
_reflns_number_total             6910
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc01611d2.cif
_cod_data_source_block           AlOC-195-Tb
_cod_depositor_comments
'Adding full bibliography for 7133236--7133243.cif.'
_cod_database_code               7133243
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Al Tb C H O N'
_shelx_estimated_absorpt_t_max   0.450
_shelx_estimated_absorpt_t_min   0.252
_reflns_odcompleteness_completeness 86.46
_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
 C01E-O2
 1.35 with sigma of 0.02
 O2-C01E
 1.3 with sigma of 0.02
 O00G-O2
 2.95 with sigma of 0.01
3. Restrained planarity
 O01G, C01E, N019, C01F, C3
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(O01G) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O2) \\sim Ueq, Uanis(O01G) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O007) \\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. Others
 Fixed Sof: H01Z(0.8) H(0.2) O01G(0.8) O2(0.2)
6.a Secondary CH2 refined with riding coordinates:
 C00P(H00A,H00B), C00Q(H00C,H00D), C00R(H00E,H00F), C00T(H00J,H00K), C00U(H00L,
 H00M), C00W(H00N,H00O), C00X(H00P,H00Q), C00Z(H00R,H00S), C012(H01A,H01B),
 C013(H01C,H01D), C014(H01E,H01F), C015(H01G,H01H), C016(H01I,H01J), C017(H01K,
 H01L), C018(H01M,H01N), C01A(H01O,H01P)
6.b Aromatic/amide H refined with riding coordinates:
 C00V(H00V), C00Y(H00Y), C010(H010), C011(H011), C01E(H01Z), C01E(H)
6.c Idealised Me refined as rotating group:
 C00S(H00G,H00H,H00I), C01B(H01Q,H01R,H01S), C01C(H01T,H01U,H01V), C01D(H01W,
 H01X,H01Y), C01F(H01,HA,HB), C3(H3A,H3B,H3C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              21104
_shelx_hkl_checksum              99585
_shelx_fab_checksum              642
_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 4.055
_oxdiff_exptl_absorpt_empirical_full_min 0.320