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_7133237
_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         '2(C96 H192 Al8 Er8 N16 O64), 8(C3 H7 N O)'
_chemical_formula_sum            'C216 H440 Al16 Er16 N40 O136'
_chemical_formula_weight         8881.89
_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                 99.049(2)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   28.9871(8)
_cell_length_b                   10.1594(3)
_cell_length_c                   27.5988(7)
_cell_measurement_reflns_used    12420
_cell_measurement_temperature    100.00(13)
_cell_measurement_theta_max      59.7400
_cell_measurement_theta_min      2.7200
_cell_volume                     8026.5(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)'
_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 0.973
_diffrn_measured_fraction_theta_max 0.973
_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   -105.00  -7.00   0.50    1.02    --  -78.59  93.00 -36.00  196
  2  \w    -68.00 -17.00   0.50    1.02    --  -78.59  38.00 -90.00  102
  3  \w   -107.00 -81.00   0.50    1.02    --  -78.59 125.00-150.00   52
  4  \w    -35.00  -4.00   0.50    0.26    --   -1.25  93.00 -36.00   62
  5  \w    -23.00  72.00   0.50    0.26    --   -1.25  57.00  30.00  190
  6  \w    -29.00  21.00   0.50    0.26    --   -1.25 -93.00-148.00  100
  7  \w   -121.00 -84.00   0.50    1.02    --  -78.59 -93.00-148.00   74
  8  \w   -130.00-104.00   0.50    1.02    --  -78.59 -99.00 -90.00   52
  9  \w   -152.00 -88.00   0.50    1.02    --  -78.59 -99.00   0.00  128
 10  \w   -151.00 -88.00   0.50    1.02    --  -78.59 -99.00 150.00  126
 11  \w     -2.00  47.00   0.50    1.02    --   76.09 -38.00-120.00   98
 12  \w      0.00  70.00   0.50    1.02    --   76.09 -38.00-150.00  140
 13  \w     29.00  54.00   0.50    1.02    --   76.09 -93.00-148.00   50
 14  \w     43.00  93.00   0.50    1.02    --   76.09 -57.00 120.00  100
 15  \w     94.00 119.00   0.50    1.02    --   76.09  93.00 -36.00   50
 16  \w     80.00 148.00   0.50    1.02    --   76.09 125.00-120.00  136
 17  \w     80.00 132.00   0.50    1.02    --   76.09 125.00  90.00  104
;
_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      -0.0452415000
_diffrn_orient_matrix_UB_12      -0.0054237000
_diffrn_orient_matrix_UB_13      0.0046825000
_diffrn_orient_matrix_UB_21      -0.0028329000
_diffrn_orient_matrix_UB_22      -0.1216519000
_diffrn_orient_matrix_UB_23      -0.0190100000
_diffrn_orient_matrix_UB_31      0.0115254000
_diffrn_orient_matrix_UB_32      -0.0505122000
_diffrn_orient_matrix_UB_33      0.0450717000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.0739
_diffrn_reflns_av_unetI/netI     0.0630
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            23628
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        52.931
_diffrn_reflns_theta_max         52.931
_diffrn_reflns_theta_min         2.819
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    14.208
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39987
_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    1.838
_exptl_crystal_description       block
_exptl_crystal_F_000             4400
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.925
_refine_diff_density_min         -0.966
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     484
_refine_ls_number_reflns         6902
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0830
_refine_ls_R_factor_gt           0.0629
_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^)+(0.0644P)^2^+141.3275P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1356
_refine_ls_wR_factor_ref         0.1457
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5593
_reflns_number_total             6902
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc01611d2.cif
_cod_data_source_block           AlOC-195-Er
_cod_depositor_comments
'Adding full bibliography for 7133236--7133243.cif.'
_cod_database_code               7133237
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Al Er C H O N'
_shelx_estimated_absorpt_t_max   0.871
_shelx_estimated_absorpt_t_min   0.436
_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 planarity
 O01F, C01E, N013, C01H, C01I
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
Uanis(C01A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O00F) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C01I) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C01H) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O01F) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Secondary CH2 refined with riding coordinates:
 C00Q(H00D,H00E), C00R(H00F,H00G), C00S(H00H,H00I), C00T(H00J,H00K), C00V(H00L,
 H00M), C00Y(H00N,H00O), C00Z(H00P,H00Q), C011(H01A,H01B), C012(H01C,H01D),
 C014(H01E,H01F), C015(H01G,H01H), C016(H01I,H01J), C017(H01K,H01L), C018(H01M,
 H01N), C01A(H01R,H01S), C01D(H01Z,H)
4.b Aromatic/amide H refined with riding coordinates:
 C00U(H00U), C00W(H00W), C00X(H00X), C010(H010), C01E(H01)
4.c Idealised Me refined as rotating group:
 C00P(H00A,H00B,H00C), C019(H01O,H01P,H01Q), C01B(H01T,H01U,H01V), C01C(H01W,
 H01X,H01Y), C01H(H0AA,HA,HB), C01I(H1AA,HC,HD)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              3872
_shelx_hkl_checksum              52940
_shelx_fab_checksum              689
_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 5.254
_oxdiff_exptl_absorpt_empirical_full_min 0.457