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_7714934
_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                   10.4466(4)
_cell_length_b                   14.3125(6)
_cell_length_c                   14.7885(7)
_cell_measurement_reflns_used    5717
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      26.33
_cell_measurement_theta_min      2.39
_cell_volume                     2211.13(16)
_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      153.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0322
_diffrn_reflns_av_unetI/netI     0.0401
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_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       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10956
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.010
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         1.980
_exptl_absorpt_coefficient_mu    1.652
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5989
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0649 before and 0.0557 after correction.
The Ratio of minimum to maximum transmission is 0.8035.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.637
_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         0.335
_refine_diff_density_min         -0.258
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details
;
 Flack x determined using 1345 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.003(13)
_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     256
_refine_ls_number_reflns         3887
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0276
_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^)+(0.0191P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0508
_refine_ls_wR_factor_ref         0.0545
_reflns_Friedel_coverage         0.745
_reflns_Friedel_fraction_full    0.989
_reflns_Friedel_fraction_max     0.989
_reflns_number_gt                3455
_reflns_number_total             3887
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03838f2.cif
_cod_data_source_block           ww
_cod_depositor_comments
'Adding full bibliography for 7714934--7714936.cif.'
_cod_database_code               7714934
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.866
_shelx_estimated_absorpt_t_min   0.839
_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. Uiso/Uaniso restraints and constraints
Uanis(C8A) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C7A) \\sim Ueq, Uanis(C7)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=1-FVAR(1)
 Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(C7)=Sof(H7A)=Sof(H7B)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C9(H9A,H9B), C3(H3A,H3B), C1(H1A,H1B), C4(H4A,H4B), C10(H10A,
 H10B), C5(H5A,H5B), C6(H6A,H6B), C8(H8A,H8B), C7(H7A,H7B), C8A(H8AA,H8AB),
 C7A(H7AA,H7AB)
4.b Aromatic/amide H refined with riding coordinates:
 C11(H11)
4.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C)
;
_shelx_res_checksum              59708
_shelx_hkl_checksum              599
_olex2_submission_special_instructions 'No special instructions were received'