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_1558404
_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         '0.5(Cl12 I16 Mo12), 3(C48 H56 O40), 17(O)'
_chemical_formula_sum            'C144 H168 Cl6 I8 Mo6 O138'
_chemical_formula_weight         5910.31
_space_group_crystal_system      tetragonal
_space_group_IT_number           97
_space_group_name_Hall           'I 4 2'
_space_group_name_H-M_alt        'I 4 2 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-03-01
_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                90
_cell_formula_units_Z            4
_cell_length_a                   23.7708(16)
_cell_length_b                   23.7708(16)
_cell_length_c                   57.456(4)
_cell_measurement_reflns_used    9875
_cell_measurement_temperature    200
_cell_measurement_theta_max      28.1
_cell_measurement_theta_min      2.33
_cell_volume                     32466(4)
_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      200.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'bruker D8 Advance'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1173
_diffrn_reflns_av_unetI/netI     0.0384
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       72
_diffrn_reflns_limit_l_min       -71
_diffrn_reflns_number            477901
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.508
_diffrn_reflns_theta_min         0.709
_exptl_absorpt_coefficient_mu    1.111
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.209
_exptl_crystal_description       plate
_exptl_crystal_F_000             11656
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.814
_refine_diff_density_min         -1.759
_refine_diff_density_rms         0.278
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.26(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         16718
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.1493
_refine_ls_R_factor_gt           0.1108
_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^)+(0.1865P)^2^+705.9324P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2881
_refine_ls_wR_factor_ref         0.3443
_reflns_Friedel_coverage         0.823
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.989
_reflns_number_gt                12659
_reflns_number_total             16718
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0mh00637h2.cif
_cod_data_source_block           iaa364_0m
_cod_depositor_comments
;Adding full bibliography for 1558402--1558407.cif.

 Adding full bibliography for 1558402--1558407.cif.
;
_cod_original_cell_volume        32465(5)
_cod_database_code               1558404
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.851
_shelx_estimated_absorpt_t_min   0.769
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.74(5)
 0.26(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Restrained distances
 Mo1-Cl3
 2.45 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C20) \\sim Ueq, Uanis(O18) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(O11)
\\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.05
Uanis(Cl3) = Uanis(Cl1) = Uanis(Cl2)
Uanis(C25) = Uanis(O27) = Uanis(C36) = Uanis(O28) = Uanis(C29) = Uanis(C28) =
Uanis(C27) = Uanis(C26) = Uanis(O26) = Uanis(O29) = Uanis(O25) = Uanis(O23) =
Uanis(C30) = Uanis(C31) = Uanis(O24) = Uanis(C32) = Uanis(O21) = Uanis(C33) =
Uanis(C34) = Uanis(C35) = Uanis(O20) = Uanis(O22)
Uanis(O10) = Uanis(C15) = Uanis(C16) = Uanis(O12) = Uanis(O13) = Uanis(C17) =
Uanis(C18) = Uanis(O14) = Uanis(C14) = Uanis(C13) = Uanis(O11) = Uanis(C21) =
Uanis(O15) = Uanis(C22) = Uanis(O16) = Uanis(C23) = Uanis(O19) = Uanis(C24) =
Uanis(O18) = Uanis(C20) = Uanis(C19) = Uanis(O17)
Uanis(O1) = Uanis(C1) = Uanis(C2) = Uanis(O2) = Uanis(C3) = Uanis(O3) =
Uanis(C4) = Uanis(O4) = Uanis(O5) = Uanis(C6) = Uanis(C7) = Uanis(C8) =
Uanis(C9) = Uanis(O6) = Uanis(O7) = Uanis(C10) = Uanis(O8) = Uanis(C11) =
Uanis(C12) = Uanis(O9) = Uanis(O30) = Uanis(C5)
5. Others
 Fixed Sof: I3(0.5) I4(0.5) I2(0.5) I1(0.5) Mo2(0.5) Mo3(0.5) Mo1(0.5)
 Cl1(0.5) O1W(0.25) Cl2(0.5) Cl3(0.5)
6.a Ternary CH refined with riding coordinates:
 C30(H30), C11(H11), C34(H34), C22(H22), C7(H7), C33(H33), C10(H10), C32(H32),
 C17(H17), C21(H21), C8(H8), C14(H14), C2(H2), C1(H1), C26(H26), C6(H6),
 C18(H18), C31(H31), C24(H24), C3(H3), C23(H23), C15(H15), C4(H4), C27(H27),
 C20(H20), C25(H25), C28(H28), C5(H5), C16(H16), C29(H29)
6.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C35(H35A,H35B), C12(H12A,H12B), C19(H19B,H19A), C9(H9A,H9B),
 C36(H36A,H36B)
;
_olex2_submission_special_instructions 'No special instructions were received'