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_7133241
_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 H94 Al4 Ho4 N8 O32, 2(C3 H7 N O), [+ solvents]'
_chemical_formula_sum            'C51 H101 Al4 Ho4 N9 O33'
_chemical_formula_weight         2136.04
_chemical_name_systematic        AlOC-195-Ho
_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             2024-06-03
_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                 99.140(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.9677(8)
_cell_length_b                   10.1285(3)
_cell_length_c                   27.6700(10)
_cell_measurement_reflns_used    9334
_cell_measurement_temperature    100.00(12)
_cell_measurement_theta_max      59.7120
_cell_measurement_theta_min      2.7320
_cell_volume                     8015.3(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  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(12)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_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      6.00  31.00   0.50    1.62    --   76.09 -99.00 -90.00   50
  2  \w     63.00  90.00   0.50    1.62    --   76.09 -99.00 -90.00   54
  3  \w     34.00  59.00   0.50    1.62    --   76.09 -37.00 -55.00   50
  4  \w     59.00  89.00   0.50    1.62    --   76.09  37.00  99.00   60
  5  \w    105.00 131.00   0.50    1.62    --   76.09  37.00  99.00   52
  6  \w     94.00 146.00   0.50    1.62    --   76.09 125.00 -30.00  104
  7  \w    -23.00  78.00   0.50    0.41    --   -1.25  37.00  99.00  202
  8  \w    -91.00 -21.00   0.50    1.62    --  -78.59 125.00  90.00  140
  9  \w    -91.00  -4.00   0.50    1.62    --  -78.59  57.00  90.00  174
 10  \w    -69.00 -34.00   0.50    1.62    --  -78.59  37.00  99.00   70
 11  \w    -56.00 -22.00   0.50    1.62    --  -78.59  38.00 -60.00   68
 12  \w    -66.00 -17.00   0.50    0.41    --   -1.25 -37.00 -55.00   98
 13  \w     -8.00  38.00   0.50    0.41    --   -1.25 -99.00-180.00   92
 14  \w   -157.00 -53.00   0.50    1.62    --  -78.59 -37.00 -55.00  208
 15  \w   -149.00-122.00   0.50    1.62    --  -78.59-125.00-180.00   54
 16  \w   -151.00 -79.00   0.50    1.62    --  -78.59-125.00  60.00  144
;
_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      -0.0377867000
_diffrn_orient_matrix_UB_12      -0.0565891000
_diffrn_orient_matrix_UB_13      -0.0259849000
_diffrn_orient_matrix_UB_21      -0.0170284000
_diffrn_orient_matrix_UB_22      -0.0241792000
_diffrn_orient_matrix_UB_23      0.0413624000
_diffrn_orient_matrix_UB_31      -0.0217922000
_diffrn_orient_matrix_UB_32      0.1170605000
_diffrn_orient_matrix_UB_33      -0.0039993000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.1331
_diffrn_reflns_av_unetI/netI     0.0992
_diffrn_reflns_Laue_measured_fraction_full 0.963
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            20049
_diffrn_reflns_point_group_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        52.931
_diffrn_reflns_theta_max         52.931
_diffrn_reflns_theta_min         2.686
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    18.304
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.21266
_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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.770
_exptl_crystal_description       block
_exptl_crystal_F_000             4216
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.834
_refine_diff_density_min         -2.042
_refine_diff_density_rms         0.362
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     484
_refine_ls_number_reflns         6816
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.1687
_refine_ls_R_factor_gt           0.1298
_refine_ls_shift/su_max          0.040
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1738P)^2^+958.0886P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3124
_refine_ls_wR_factor_ref         0.3467
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4901
_reflns_number_total             6816
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc01611d2.cif
_cod_data_source_block           AlOC-195-Ho
_cod_depositor_comments
'Adding full bibliography for 7133236--7133243.cif.'
_cod_database_code               7133241
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Al Ho C H O N'
_shelx_estimated_absorpt_t_max   0.461
_shelx_estimated_absorpt_t_min   0.262
_reflns_odcompleteness_completeness 95.86
_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(C018) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N01F) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C17) \\sim Ueq, Uanis(O01E) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C00Y) \\sim Ueq, Uanis(C012) \\sim Ueq, Uanis(C00O) \\sim Ueq: with sigma
of 0.1 and sigma for terminal atoms of 0.2
Uanis(C016) \\sim Ueq, Uanis(C00Y) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O00C) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C01A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C017) \\sim Ueq, Uanis(C01A) \\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(C014) \\sim Ueq, Uanis(C010) \\sim Ueq, Uanis(C01D) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C29) \\sim Ueq, Uanis(C23) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3. Others
 Fixed Sof: O01E(0.5) N01F(0.5) C17(0.5) H17(0.5) C23(0.5) H23A(0.5) H23B(0.5)
 H23C(0.5) C29(0.5) H29A(0.5) H29B(0.5) H29C(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C00O(H00A,H00B), C00Q(H00C,H00D), C00R(H00E,H00F), C00S(H00G,H00H), C00W(H00L,
 H00M), C00X(H00N,H00O), C00Z(H00P,H00Q), C010(H01A,H01B), C011(H01C,H01D),
 C012(H01E,H01F), C014(H01G,H01H), C015(H01I,H01J), C016(H01K,H01L), C018(H01P,
 H01Q), C01A(H01U,H01V)
4.b Aromatic/amide H refined with riding coordinates:
 C00T(H00T), C00V(H00V), C00Y(H00Y), C013(H013), C01B(H01W), C17(H17)
4.c Idealised Me refined as rotating group:
 C00U(H00I,H00J,H00K), C017(H01M,H01N,H01O), C019(H01R,H01S,H01T), C01D(H01X,
 H01Y,H), C23(H23A,H23B,H23C), C29(H29A,H29B,H29C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              10547
_shelx_hkl_checksum              51839
_shelx_fab_checksum              34742
_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 6.085
_oxdiff_exptl_absorpt_empirical_full_min 0.205