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_1558407
_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
'Br8 Cl6 Mo6, C96 H112 Na5 O94.5, 2(Cl), 8(O)'
_chemical_formula_sum            'C96 H112 Br8 Cl8 Mo6 Na5 O102.5'
_chemical_formula_weight         4519.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_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                 93.734(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.8501(17)
_cell_length_b                   32.821(4)
_cell_length_c                   17.405(2)
_cell_measurement_reflns_used    9416
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.506
_cell_measurement_theta_min      2.426
_cell_volume                     9035.1(18)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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      150.15
_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  0.0347
_diffrn_reflns_av_unetI/netI     0.0565
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            113359
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.525
_diffrn_reflns_theta_min         2.092
_exptl_absorpt_coefficient_mu    2.402
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5890
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1115 before and 0.0706 after correction. The Ratio of minimum to maximum transmission is 0.7900. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.661
_exptl_crystal_description       plate
_exptl_crystal_F_000             4462
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.586
_refine_diff_density_min         -1.380
_refine_diff_density_rms         0.192
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.028(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2109
_refine_ls_number_reflns         40804
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0593
_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^)+(0.1079P)^2^+38.2915P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1701
_refine_ls_wR_factor_ref         0.1817
_reflns_Friedel_coverage         0.929
_reflns_Friedel_fraction_full    0.962
_reflns_Friedel_fraction_max     0.960
_reflns_number_gt                34744
_reflns_number_total             40804
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0mh00637h2.cif
_cod_data_source_block           import_a
_cod_depositor_comments
;Adding full bibliography for 1558402--1558407.cif.

 Adding full bibliography for 1558402--1558407.cif.
;
_cod_original_cell_volume        9035.4(18)
_cod_original_formula_sum        'C96 H112 Br8 Cl8 Mo6 Na5 O102.50'
_cod_database_code               1558407
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.931
_shelx_estimated_absorpt_t_min   0.514
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.972(8)
 0.028(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(O1) \\sim Ueq, Uanis(O12W) \\sim Ueq, Uanis(O14) \\sim Ueq, Uanis(O27)
\\sim Ueq, Uanis(O33W) \\sim Ueq, Uanis(O18W) \\sim Ueq: with sigma of 0.001
and sigma for terminal atoms of 0.002
Uanis(O40) = Uanis(C48) = Uanis(C47)
4. Others
 Fixed Sof: Na8(0.5) O1W(0.5) Na2(0.5) O23W(0.5) O8W(0.5) O13W(0.5) O34W(0.5)
 Na7(0.5) O27W(0.5) O12W(0.5) O15W(0.5) O18W(0.5) O10W(0.5) O16W(0.5) O25W(0.5)
 O4W(0.5) O28W(0.5) Na5(0.5) Na6(0.5) O0AA(0.5) Na4(0.5)
5.a Ternary CH refined with riding coordinates:
 C94(H94), C89(H89), C66(H66), C53(H53), C1(H1), C93(H93), C3(H3), C7(H7),
 C54(H54), C14(H14), C45(H45), C60(H60), C47(H47), C33(H33), C75(H75), C70(H70),
  C19(H19), C27(H27), C64(H64), C2(H2), C20(H20), C96(H96), C95(H95), C9(H9),
 C76(H76), C43(H43), C21(H21), C88(H88), C77(H77), C26(H26), C50(H50), C39(H39),
  C28(H28), C92(H92), C84(H84), C34(H34), C25(H25), C4(H4), C5(H5), C78(H78),
 C63(H63), C80(H80), C87(H87), C29(H29), C17(H17), C44(H44), C15(H15), C52(H52),
  C74(H74), C10(H10), C41(H41), C8(H8), C22(H22), C82(H82), C16(H16), C71(H71),
 C51(H51), C58(H58), C11(H11), C32(H32), C57(H57), C69(H69), C90(H90), C13(H13),
  C46(H46), C31(H31), C83(H83), C56(H56), C86(H86), C40(H40), C59(H59),
 C68(H68), C37(H37), C81(H81), C35(H35), C62(H62), C38(H38), C23(H23), C65(H65),
  C72(H72)
5.b Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C55(H55A,H55B), C85(H85A,H85B), C61(H61A,H61B), C12(H12A,
 H12B), C49(H49A,H49B), C24(H24A,H24B), C18(H18A,H18B), C48(H48A,H48B), C6(H6A,
 H6B), C36(H36A,H36B), C73(H73A,H73B), C91(H91A,H91B), C42(H42A,H42B), C79(H79A,
 H79B), C67(H67A,H67B)
;
_olex2_submission_special_instructions 'No special instructions were received'