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_7133239
_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(C95.97 H191.95 Al8 Gd8 N16 O64)'
_chemical_formula_sum            'C47.99 H95.97 Al4 Gd4 N8 O32'
_chemical_formula_weight         2034.06
_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   mixed
_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                 117.751(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.5463(7)
_cell_length_b                   10.2945(2)
_cell_length_c                   29.7052(8)
_cell_measurement_reflns_used    12335
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      60.1460
_cell_measurement_theta_min      3.1350
_cell_volume                     7454.8(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      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 0.975
_diffrn_measured_fraction_theta_max 0.975
_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     51.00  77.00   0.50    0.65    --   77.36-125.00-180.00   52
  2  \w     12.00  37.00   0.50    0.65    --   77.36 -41.00-140.00   50
  3  \w     80.00 149.00   0.50    0.65    --   77.36 125.00  30.00  138
  4  \w     79.00 104.00   0.50    0.65    --   77.36  41.00  11.00   50
  5  \w     -1.00  71.00   0.50    0.65    --   77.36 -38.00 120.00  144
  6  \w    -24.00  76.00   0.50    0.15    --   -0.55  41.00  11.00  200
  7  \w    -68.00   0.00   0.50    0.65    --  -78.46  38.00 120.00  136
  8  \w    -72.00   0.00   0.50    0.65    --  -78.46  41.00  11.00  144
  9  \w    -41.00  -8.00   0.50    0.65    --  -78.46  38.00-180.00   66
 10  \w    -68.00 -13.00   0.50    0.15    --   -0.55 -41.00-140.00  110
 11  \w   -156.00 -93.00   0.50    0.65    --  -78.46 -41.00-140.00  126
 12  \w    -55.00 -30.00   0.50    0.65    --  -78.46 125.00 120.00   50
 13  \w   -109.00 -62.00   0.50    0.65    --  -78.46 125.00 120.00   94
 14  \w    -71.00 -41.00   0.50    0.15    --   -0.55 -57.00 -90.00   60
 15  \w     -8.00  17.00   0.50    0.15    --   -0.55 -99.00-180.00   50
 16  \w   -147.00-121.00   0.50    0.65    --  -78.46-125.00   0.00   52
 17  \w   -118.00 -80.00   0.50    0.65    --  -78.46-125.00   0.00   76
 18  \w   -150.00-119.00   0.50    0.65    --  -78.46 -99.00 150.00   62
;
_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      0.0393797000
_diffrn_orient_matrix_UB_12      0.0293245000
_diffrn_orient_matrix_UB_13      0.0467466000
_diffrn_orient_matrix_UB_21      -0.0282706000
_diffrn_orient_matrix_UB_22      -0.0610369000
_diffrn_orient_matrix_UB_23      0.0201857000
_diffrn_orient_matrix_UB_31      0.0258406000
_diffrn_orient_matrix_UB_32      -0.1110775000
_diffrn_orient_matrix_UB_33      0.0012303000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.0776
_diffrn_reflns_av_unetI/netI     0.0742
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            22513
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        52.925
_diffrn_reflns_theta_max         52.925
_diffrn_reflns_theta_min         4.009
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    19.574
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42934
_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    1.812
_exptl_crystal_description       block
_exptl_crystal_F_000             4016
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.335
_refine_diff_density_min         -0.995
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     498
_refine_ls_number_reflns         6430
_refine_ls_number_restraints     92
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0440
_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^)+(0.0529P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0990
_refine_ls_wR_factor_ref         0.1065
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5058
_reflns_number_total             6430
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc01611d2.cif
_cod_data_source_block           AlOC-195-Gd
_cod_depositor_comments
'Adding full bibliography for 7133236--7133243.cif.'
_cod_database_code               7133239
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.245
_shelx_estimated_absorpt_t_min   0.245
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     56.82
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H00A,H00B,H00C} of C00P, All C(H,H) groups, All C(H,H,H,
  H) groups
 At 1.5 times of:
  {H01T,H01U,H01V} of C019, {H01K,H01L,H01M} of C015, {H00L,H00M,H00N} of C00X
2. Restrained distances
 N00O-C01B
 1.43 with sigma of 0.02
 C01B-C3
 1.4 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C01B) \\sim Ueq, Uanis(C01A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C01D) \\sim Ueq, Uanis(C018) \\sim Ueq, Uanis(C016) \\sim Ueq,
Uanis(C017) \\sim Ueq, Uanis(C01A) \\sim Ueq, Uanis(C019) \\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(C01D) \\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(C2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C011) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C01A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C01D) \\sim Ueq, Uanis(C018) \\sim Ueq, Uanis(C014) \\sim Ueq,
Uanis(C017) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C014) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C8) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C015) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C015) \\sim Ueq, Uanis(C014) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Fixed Sof: H01C(0.5) H01D(0.5) H01E(0.5) H01F(0.5) C014(0.8) H01I(0.8)
 H01J(0.8) C016(0.6) H01N(0.6) H01O(0.6) C017(0.5) H01P(0.5) H01Q(0.5)
 C018(0.5) H01R(0.5) H01S(0.5) C01A(0.6) H01W(0.6) H01X(0.6) C01D(0.66)
 H01Y(0.66) H(0.66) C1(0.5) H1A(0.5) H1B(0.5) C2(0.4) H2A(0.4) H2B(0.4)
 C3(0.33333) H3A(0.33333) H3B(0.33333) C4(0.5) H4A(0.5) H4B(0.5) C5(0.5)
 H5A(0.5) H5B(0.5) C6(0.5) H6A(0.5) H6B(0.5) C01B(0.4) H01Z(0.4) HA(0.4)
 C8(0.2) H8A(0.2) H8B(0.2)
5.a Riding coordinates:
 C014(H01I,H01J), C015(H01K,H01L,H01M), C016(H01N,H01O), C019(H01T,H01U,H01V),
 C4(H4A,H4B), C01B(H01Z,HA), C8(H8A,H8B)
5.b Secondary CH2 refined with riding coordinates:
 C00R(H00D,H00E), C00T(H00F,H00G), C00V(H00H,H00I), C00W(H00J,H00K), C00Y(H00O,
 H00P), C00Z(H00R,H00T), C010(H01A,H01B), C011(H01C,H01D), C011(H01E,H01F),
 C012(H01G,H01H), C017(H01P,H01Q), C018(H01R,H01S), C01A(H01W,H01X), C01D(H01Y,
 H), C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C5(H5A,H5B), C6(H6A,H6B)
5.c Aromatic/amide H refined with riding coordinates:
 C00Q(H00Q), C00S(H00S), C00U(H00U), C013(H013)
5.d Idealised Me refined as rotating group:
 C00P(H00A,H00B,H00C), C00X(H00L,H00M,H00N)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              22622
_shelx_hkl_checksum              79991
_shelx_fab_checksum              10833
_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 2.617
_oxdiff_exptl_absorpt_empirical_full_min 0.422