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_1558402
_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
'Cl6 I8 Mo6, 2(Cl), C96 H112 Na4.5 O92.5, 14.5(O)'
_chemical_formula_sum            'C96 H112 Cl8 I8 Mo6 Na4.5 O107'
_chemical_formula_weight         4955.74
_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                 93.728(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.8187(9)
_cell_length_b                   32.856(2)
_cell_length_c                   17.4013(11)
_cell_measurement_reflns_used    5401
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.2
_cell_measurement_theta_min      1.8
_cell_volume                     9025.0(9)
_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(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'bruker D8 Advance'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0717
_diffrn_reflns_av_unetI/netI     0.0620
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -20
_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            238942
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.142
_diffrn_reflns_theta_min         1.799
_exptl_absorpt_coefficient_mu    2.004
_exptl_absorpt_correction_T_max  0.942
_exptl_absorpt_correction_T_min  0.690
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.824
_exptl_crystal_description       plate
_exptl_crystal_F_000             4811
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.438
_refine_diff_density_min         -1.169
_refine_diff_density_rms         0.201
_refine_ls_abs_structure_details
;
 Flack x determined using 12466 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.013(5)
_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     1984
_refine_ls_number_reflns         39940
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0755
_refine_ls_R_factor_gt           0.0484
_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^)+(0.0716P)^2^+32.5819P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1230
_refine_ls_wR_factor_ref         0.1423
_reflns_Friedel_coverage         0.964
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                30546
_reflns_number_total             39940
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0mh00637h2.cif
_cod_data_source_block           import
_cod_depositor_comments
;Adding full bibliography for 1558402--1558407.cif.

 Adding full bibliography for 1558402--1558407.cif.
;
_cod_original_formula_sum        'C96 H112 Cl8 I8 Mo6 Na4.50 O107'
_cod_database_code               1558402
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.942
_shelx_estimated_absorpt_t_min   0.690
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C36) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O27) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O25) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: Cl7(0.5) Cl8(0.5) Na3(0.5) Na4(0.5) Na5(0.5) O7W(0.5) O94(0.5)
 O6W(0.5) O25W(0.5) O8W(0.5) O103(0.5) O104(0.5) O22W(0.5) O17W(0.5) O107(0.5)
 O4W(0.5) O5W(0.5) O9W(0.5) O15W(0.5) O31W(0.5) O23W(0.5) O3W(0.5) O20W(0.25)
 O21W(0.25)
4.a Ternary CH refined with riding coordinates:
 C33(H33), C29(H29), C63(H63), C45(H45), C39(H39), C15(H15), C96(H96),
 C82(H82), C94(H94), C14(H14), C54(H54), C91(H91), C95(H95), C25(H25), C43(H43),
  C38(H38), C76(H76), C22(H22), C9(H9), C74(H74), C66(H66), C47(H47), C79(H79),
 C93(H93), C85(H85), C7(H7), C81(H81), C8(H8), C53(H53), C50(H50), C41(H41),
 C75(H75), C21(H21), C23(H23), C2(H2), C52(H52), C32(H32), C62(H62), C57(H57),
 C34(H34), C59(H59), C35(H35), C83(H83), C27(H27), C28(H28), C78(H78), C51(H51),
  C10(H10), C73(H73), C44(H44), C46(H46), C13(H13), C16(H16), C69(H69),
 C11(H11), C90(H90), C89(H89), C60(H60), C88(H88), C3(H3), C58(H58), C4(H4),
 C37(H37), C87(H87), C20(H20), C40(H40), C31(H31), C68(H68), C56(H56), C26(H26),
  C1(H1), C64(H64), C19(H19), C61(H61), C17(H17), C86(H86), C67(H67), C5(H5),
 C77(H77), C70(H70)
4.b Secondary CH2 refined with riding coordinates:
 C48(H48A,H48B), C12(H12A,H12B), C71(H71A,H71B), C18(H18A,H18B), C65(H65A,
 H65B), C92(H92A,H92B), C55(H55A,H55B), C80(H80A,H80B), C42(H42A,H42B),
 C30(H30A,H30B), C24(H24A,H24B), C49(H49A,H49B), C6(H6A,H6B), C72(H72A,H72B),
 C36(H36A,H36B), C84(H84A,H84B)
;
_olex2_submission_special_instructions 'No special instructions were received'