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_7133238
_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 Sm4'
_chemical_formula_sum            'C48 H96 Al4 N8 O32 Sm4'
_chemical_formula_weight         2006.64
_chemical_name_systematic        AlOC-195-Sm
_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
_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                 118.087(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.9072(5)
_cell_length_b                   10.2096(2)
_cell_length_c                   29.8833(6)
_cell_measurement_reflns_used    14543
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      59.9640
_cell_measurement_theta_min      2.6390
_cell_volume                     7511.7(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 0.981
_diffrn_measured_fraction_theta_max 0.981
_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     79.00 105.00   0.50    0.05    --   75.78 125.00-120.00   52
  2  \w    115.00 145.00   0.50    0.05    --   75.78 125.00-120.00   60
  3  \w     96.00 155.00   0.50    0.05    --   75.78  38.00 150.00  118
  4  \w     95.00 120.00   0.50    0.05    --   75.78 100.00 156.00   50
  5  \w    -71.00 -15.00   0.50    0.05    --  -78.59  38.00   0.00  112
  6  \w    -89.00 -64.00   0.50    0.05    --  -78.59 125.00   0.00   50
  7  \w   -105.00 -13.00   0.50    0.05    --  -78.59 100.00 156.00  184
  8  \w    -18.00  56.00   0.50    0.05    --   -1.41  57.00  30.00  148
  9  \w    -41.00 -16.00   0.50    0.05    --   -1.41 100.00 156.00   50
 10  \w     15.00  65.00   0.50    0.05    --   75.78 -38.00  90.00  100
 11  \w     12.00  86.00   0.50    0.05    --   75.78-100.00  51.00  148
 12  \w     -6.00  33.00   0.50    0.05    --   -1.41 -99.00 -90.00   78
 13  \w     -8.00  19.00   0.50    0.05    --   -1.41-100.00  51.00   54
 14  \w   -121.00 -91.00   0.50    0.05    --  -78.59-100.00  51.00   60
 15  \w   -149.00 -82.00   0.50    0.05    --  -78.59-125.00 -30.00  134
 16  \w   -153.00-104.00   0.50    0.05    --  -78.59 -99.00 -60.00   98
 17  \w   -150.00 -88.00   0.50    0.05    --  -78.59 -99.00-150.00  124
;
_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      0.0054538000
_diffrn_orient_matrix_UB_12      -0.0313532000
_diffrn_orient_matrix_UB_13      0.0456695000
_diffrn_orient_matrix_UB_21      -0.0158309000
_diffrn_orient_matrix_UB_22      0.1208346000
_diffrn_orient_matrix_UB_23      0.0045962000
_diffrn_orient_matrix_UB_31      -0.0517649000
_diffrn_orient_matrix_UB_32      -0.0403131000
_diffrn_orient_matrix_UB_33      -0.0217526000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.0862
_diffrn_reflns_av_unetI/netI     0.0655
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            21872
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        52.932
_diffrn_reflns_theta_max         52.932
_diffrn_reflns_theta_min         2.915
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    16.705
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.13546
_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 yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.774
_exptl_crystal_description       block
_exptl_crystal_F_000             3984
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.849
_refine_diff_density_min         -1.222
_refine_diff_density_rms         0.204
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     462
_refine_ls_number_reflns         6511
_refine_ls_number_restraints     127
_refine_ls_restrained_S_all      1.340
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0571
_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^)+(0.1046P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1469
_refine_ls_wR_factor_ref         0.1526
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5521
_reflns_number_total             6511
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc01611d2.cif
_cod_data_source_block           AlOC-195-Sm
_cod_depositor_comments
'Adding full bibliography for 7133236--7133243.cif.'
_cod_database_code               7133238
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Al Sm C H O N'
_shelx_estimated_absorpt_t_max   0.286
_shelx_estimated_absorpt_t_min   0.026
_reflns_odcompleteness_completeness 99.68
_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, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C00Z-N00L = C00Z-C013
 1 with sigma of 0.02
 C00Z-C013
 1.46 with sigma of 0.01
 N00L-Sm01 = N00L-C00X = N00L-C00Z = N00L-C012
 1.42 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C01D) \\sim Ueq, Uanis(C01C) \\sim Ueq, Uanis(C01B) \\sim Ueq,
Uanis(C010) \\sim Ueq, Uanis(C015) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C0) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C01C) \\sim Ueq, Uanis(C01D) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C018) \\sim Ueq, Uanis(C01A) \\sim Ueq, Uanis(C016) \\sim Ueq: with sigma
of 0.1 and sigma for terminal atoms of 0.2
Uanis(C01A) \\sim Ueq, Uanis(C018) \\sim Ueq, Uanis(C016) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C00X) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C019) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C01E) \\sim Ueq, Uanis(C01D) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(Sm01) \\sim Ueq, Uanis(Sm02) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(C013) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C014) \\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(C018) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O00H) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C00Z) \\sim Ueq, Uanis(N00L) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Fixed Sof: H01L(0.55) H01M(0.55) H01N(0.45) H01O(0.45) C018(0.55) H01P(0.55)
 H01Q(0.55) C019(0.5) H01R(0.5) H01S(0.5) C01A(0.45) H01T(0.45) H01U(0.45)
 H01Y(0.5) H(0.5) HA(0.5) HB(0.5) C01D(0.5) H01Z(0.5) HC(0.5) C01E(0.5)
 H01(0.5) HD(0.5) H1AA(0.5) H1AB(0.5) H1BC(0.5) H1BD(0.5) C0(0.5) H0A(0.5)
 H0B(0.5)
5.a Riding coordinates:
 C00X(H00L,H00M,H00N), C011(H01C,H01D,H01E)
5.b Secondary CH2 refined with riding coordinates:
 C00P(H00A,H00B), C00T(H00F,H00G), C00U(H00H,H00I), C00V(H00J,H00K), C00Y(H00O,
 H00P), C00Z(H00R,H00T), C010(H01A,H01B), C012(H01F,H01G), C013(H01H,H01I),
 C015(H01J,H01K), C016(H01L,H01M), C016(H01N,H01O), C018(H01P,H01Q), C019(H01R,
 H01S), C01A(H01T,H01U), C01C(H01Y,H), C01C(HA,HB), C01D(H01Z,HC), C01E(H01,HD),
  C1(H1AA,H1AB), C1(H1BC,H1BD), C0(H0A,H0B)
5.c Aromatic/amide H refined with riding coordinates:
 C00Q(H00Q), C00S(H00S), C00W(H00W), C014(H014)
5.d Idealised Me refined as rotating group:
 C00R(H00C,H00D,H00E), C01B(H01V,H01W,H01X)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              40304
_shelx_hkl_checksum              21655
_shelx_fab_checksum              64988
_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 3.162
_oxdiff_exptl_absorpt_empirical_full_min 0.332