Supramolecular crystals of Mn(15-crown-5)(MnCl<sub>4</sub>)(DMF) with dielectric phase transition, high quantum yield and phase transition-induced luminescence enhancement behavior.
Yuan, Guo-Jun; Pan, Xue-Wei; Chen, Li; Chen, Chao; Ren, Xiao-Ming; Dalton transactions (Cambridge, England : 2003) 53 (2024) 2687–2695; doi:10.1039/d3dt03838f

data_7714935
_publ_section_title
;
 Supramolecular crystals of Mn(15-crown-5)(MnCl<sub>4</sub>)(DMF) with
 dielectric phase transition, high quantum yield and phase
 transition-induced luminescence enhancement behavior.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2687
_journal_page_last               2695
_journal_paper_doi               10.1039/d3dt03838f
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C13 H27 Cl4 Mn2 N O6'
_chemical_formula_sum            'C13 H27 Cl4 Mn2 N O6'
_chemical_formula_weight         545.03
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-01-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-07-14 deposited with the CCDC.	2024-01-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.2522(4)
_cell_length_b                   14.7124(7)
_cell_length_c                   15.6349(8)
_cell_measurement_reflns_used    2733
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      22.35
_cell_measurement_theta_min      2.42
_cell_volume                     2358.28(19)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_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      298
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_av_unetI/netI     0.0621
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11660
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         2.376
_exptl_absorpt_coefficient_mu    1.549
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6865
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0685 before and 0.0587 after correction.
The Ratio of minimum to maximum transmission is 0.9210.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_description       block
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.564
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details
;
 Flack x determined using 899 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.02(2)
_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     373
_refine_ls_number_reflns         4131
_refine_ls_number_restraints     764
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0876
_refine_ls_R_factor_gt           0.0517
_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^)+(0.0460P)^2^+2.2564P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1064
_refine_ls_wR_factor_ref         0.1295
_reflns_Friedel_coverage         0.750
_reflns_Friedel_fraction_full    0.989
_reflns_Friedel_fraction_max     0.989
_reflns_number_gt                2886
_reflns_number_total             4131
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03838f2.cif
_cod_data_source_block           ww_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7714934--7714936.cif.'
_cod_database_code               7714935
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.873
_shelx_estimated_absorpt_t_min   0.848
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C8-C7
 1.5 with sigma of 0.02
 O1A-C1A
 1.45 with sigma of 0.02
 C1A-C2A
 1.5 with sigma of 0.02
 O2A-C2A
 1.45 with sigma of 0.02
 O2A-C3A
 1.45 with sigma of 0.02
 C3A-C4A
 1.5 with sigma of 0.02
 C4A-O3A
 1.45 with sigma of 0.02
 O3A-C5A
 1.45 with sigma of 0.02
 C5A-C6A
 1.5 with sigma of 0.02
 O4A-C6A
 1.45 with sigma of 0.02
 O4A-C7A
 1.45 with sigma of 0.02
 C7A-C8A
 1.5 with sigma of 0.02
 C8A-O5A
 1.45 with sigma of 0.02
 O5A-C9A
 1.45 with sigma of 0.02
 C9A-C10A
 1.5 with sigma of 0.02
 C10A-O1A
 1.45 with sigma of 0.02
 Mn1-O4A
 2.1 with sigma of 0.02
 C9A-C8A
 2.35 with sigma of 0.02
 O3A-Mn1
 2.1 with sigma of 0.02
 C6A-O3A
 2.34 with sigma of 0.02
 O4A-C5A
 2.35 with sigma of 0.02
 O3A-C3A
 2.35 with sigma of 0.02
 O2A-C4A
 2.35 with sigma of 0.02
3. Rigid bond restraints
 O1, O2, O3, O4, O5, C1, C2, C3, C4, C5, C6, C7, C8, C9, C10, C3A, O2A, C2A,
 C1A, O1A, C10A, C9A, O5A, C8A, C7A, O4A, C6A, C5A, O3A, C4A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N1, C12
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N1, C13
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N1, C11
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
O1 \\sim O2 \\sim O3 \\sim O4 \\sim O5 \\sim C1 \\sim C2 \\sim C3 \\sim C4
\\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9 \\sim C10 \\sim C3A \\sim O2A
\\sim C2A \\sim C1A \\sim O1A \\sim C10A \\sim C9A \\sim O5A \\sim C8A \\sim
C7A \\sim O4A \\sim C6A \\sim C5A \\sim O3A \\sim C4A: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
Uanis(O1) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(O4) \\sim
Ueq, Uanis(O5) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3)
\\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq,
Uanis(C7) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim
Ueq, Uanis(C3A) \\sim Ueq, Uanis(O2A) \\sim Ueq, Uanis(C2A) \\sim Ueq,
Uanis(C1A) \\sim Ueq, Uanis(O1A) \\sim Ueq, Uanis(C10A) \\sim Ueq, Uanis(C9A)
\\sim Ueq, Uanis(O5A) \\sim Ueq, Uanis(C8A) \\sim Ueq, Uanis(C7A) \\sim Ueq,
Uanis(O4A) \\sim Ueq, Uanis(C6A) \\sim Ueq, Uanis(C5A) \\sim Ueq, Uanis(O3A)
\\sim Ueq, Uanis(C4A) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C12) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C11) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(O2A)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(C1A)=
 Sof(H1AA)=Sof(H1AB)=Sof(O1A)=Sof(C10A)=Sof(H10C)=Sof(H10D)=Sof(C9A)=Sof(H9AA)=
 Sof(H9AB)=Sof(O5A)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=
 Sof(O4A)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(O3A)=
 Sof(C4A)=Sof(H4AA)=Sof(H4AB)=1-FVAR(1)
 Sof(O1)=Sof(O2)=Sof(O3)=Sof(O4)=Sof(O5)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(C2)=
 Sof(H2A)=Sof(H2B)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(C5)=
 Sof(H5A)=Sof(H5B)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(C8)=
 Sof(H8A)=Sof(H8B)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(C10)=Sof(H10A)=Sof(H10B)=
 FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C3A(H3AA,H3AB),
 C2A(H2AA,H2AB), C1A(H1AA,H1AB), C10A(H10C,H10D), C9A(H9AA,H9AB), C8A(H8AA,
 H8AB), C7A(H7AA,H7AB), C6A(H6AA,H6AB), C5A(H5AA,H5AB), C4A(H4AA,H4AB)
6.b Aromatic/amide H refined with riding coordinates:
 C11(H11)
6.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C)
;
_shelx_res_checksum              11194
_shelx_hkl_checksum              48554
_olex2_submission_special_instructions 'No special instructions were received'