From supramolecular to solid state chemistry: crystal engineering of luminescent materials by trapping molecular clusters in an aluminium-based host matrix
Falaise, Clément; Ivanov, Anton A.; Molard, Yann; Amela Cortes, Maria; Shestopalov, Michael A.; Haouas, Mohamed; Cadot, Emmanuel; Cordier, Stéphane; Materials Horizons 7 (2020) 2399–2406; doi:10.1039/D0MH00637H

data_1558406
_publ_section_title
;
 From supramolecular to solid state chemistry: crystal engineering of
 luminescent materials by trapping molecular clusters in an
 aluminium-based host matrix
;
_journal_issue                   9
_journal_name_full               'Materials Horizons'
_journal_page_first              2399
_journal_page_last               2406
_journal_paper_doi               10.1039/D0MH00637H
_journal_volume                  7
_journal_year                    2020
_chemical_formula_moiety
'Cl4.5 I8 Mo6, Al13 O40, 2(C48 H54 O40), 4(Cl)'
_chemical_formula_sum            'C96 H108 Al13 Cl8.5 I8 Mo6 O120'
_chemical_formula_weight         5424.72
_space_group_crystal_system      hexagonal
_space_group_IT_number           180
_space_group_name_Hall           'P 62 2 (0 0 4)'
_space_group_name_H-M_alt        'P 62 2 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-03-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-03-02 deposited with the CCDC.	2020-06-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   19.751(2)
_cell_length_b                   19.751
_cell_length_c                   57.616(7)
_cell_measurement_reflns_used    9511
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.65
_cell_measurement_theta_min      2.43
_cell_volume                     19465(3)
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      200
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'bruker D8 Advance'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0799
_diffrn_reflns_av_unetI/netI     0.0421
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       75
_diffrn_reflns_limit_l_min       -65
_diffrn_reflns_number            189091
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.887
_diffrn_reflns_theta_min         2.062
_exptl_absorpt_coefficient_mu    1.443
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6093
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_description       block
_exptl_crystal_F_000             7900
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.13
_refine_diff_density_max         3.041
_refine_diff_density_min         -4.736
_refine_diff_density_rms         0.298
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.28(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.738
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         15487
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.741
_refine_ls_R_factor_all          0.1638
_refine_ls_R_factor_gt           0.1367
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3625
_refine_ls_wR_factor_ref         0.4039
_reflns_Friedel_coverage         0.751
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                11960
_reflns_number_total             15487
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0mh00637h2.cif
_cod_data_source_block           test
_cod_depositor_comments
;Adding full bibliography for 1558402--1558407.cif.

 Adding full bibliography for 1558402--1558407.cif.
;
_cod_original_cell_volume        19465(5)
_cod_original_sg_symbol_Hall     'P 62 2c (0 0 1)'
_cod_original_formula_sum        'C96 H108 Al13 Cl8.50 I8 Mo6 O120'
_cod_database_code               1558406
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.72(5)
 0.28(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Restrained distances
 C24A-O19A
 1.45 with sigma of 0.002
 C23A-C24A
 1.45 with sigma of 0.002
 C9A-O5A
 1.45 with sigma of 0.002
 C21A-O17A
 1.45 with sigma of 0.002
 C20A-C21A
 1.45 with sigma of 0.002
 Mo1_$2-Mo4_$3
 0.32 with sigma of 0.002
 C23A-O19A
 2.6 with sigma of 0.02
 O18A-C24A
 2.4 with sigma of 0.04
 C24A-C3A_$1
 2.6 with sigma of 0.04
 C8A-O5A
 2.6 with sigma of 0.02
 O4A-C9A
 2.4 with sigma of 0.02
 C7A-C9A
 2.6 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O19A) = Uanis(O18A) = Uanis(O15A) = Uanis(O16A) = Uanis(O13A) =
Uanis(O14A) = Uanis(O10A) = Uanis(O9A) = Uanis(O7A) = Uanis(O8A) = Uanis(O11A)
= Uanis(O17A) = Uanis(O5A) = Uanis(O4A) = Uanis(O2A) = Uanis(O3A) = Uanis(O6A)
= Uanis(O1A) = Uanis(O20A) = Uanis(O12A)
Uanis(C24A) = Uanis(C21A) = Uanis(C23A) = Uanis(C20A) = Uanis(C19A) =
Uanis(C22A) = Uanis(C17A) = Uanis(C18A) = Uanis(C16A) = Uanis(C13A) =
Uanis(C11A) = Uanis(C14A) = Uanis(C15A) = Uanis(C10A) = Uanis(C12A) =
Uanis(C9A) = Uanis(C8A) = Uanis(C7A) = Uanis(C5A) = Uanis(C6A) = Uanis(C4A) =
Uanis(C3A) = Uanis(C2A) = Uanis(C1A)
Uanis(O1) = Uanis(O4) = Uanis(O5) = Uanis(O7) = Uanis(O9) = Uanis(O8) =
Uanis(O6) = Uanis(O2) = Uanis(O3) = Uanis(O10)
Uiso(I3AA) = Uiso(I1AA) = Uiso(I0AA) = Uiso(I2AA)
Uiso(Mo4) = Uiso(Mo2A) = Uiso(Mo1) = Uiso(Mo0A)
5. Others
 Fixed Sof: I1(0.75) Mo1A(0.375) Mo3(0.75) I4AA(0.75) Cl1(0.375) Cl2(0.75)
 Mo1(0.0625) Mo4(0.0625) I0AA(0.125) I1AA(0.125) I3AA(0.125) I2AA(0.125)
 Mo2A(0.125) Mo0A(0.125)
6.a Ternary CH refined with riding coordinates:
 C11A(H11A), C12A(H12A), C10A(H10A), C14A(H14A), C13A(H13A), C6A(H6A),
 C7A(H7A), C4A(H4A), C5A(H5A), C16A(H16A), C17A(H13B), C19A(H19A), C18A(H18A),
 C1A(H1A), C2A(H2A), C8A(H8A), C22A(H22A), C20A(H20A), C23A(H23A)
6.b Secondary CH2 refined with riding coordinates:
 C15A(H15A,H15B), C21A(H21A,H21B), C9A(H9AA,H9AB), C24A(H24A,H24B)
;
_olex2_submission_special_instructions 'No special instructions were received'