Dual dielectric-responsive hybrid materials with fluorescent properties
Xu, Ran; Lun, Meng-Meng; Zhang, Tie; Li, Jie; Zou, Ke; Zhang, Yi; Fu, Da-Wei; Guo, Qiang; New Journal of Chemistry 47 (2023) 2405–2411; doi:10.1039/D2NJ04939B

data_7062174
_publ_section_title
;
 Dual dielectric-responsive hybrid materials with fluorescent properties
;
_journal_issue                   5
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              2405
_journal_page_last               2411
_journal_paper_doi               10.1039/D2NJ04939B
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety
'6(C6 H15 Br N), Br1.269 Cl2.731 Mn, 2(Br1.744 Cl2.256 Mn)'
_chemical_formula_sum            'C36 H90 Br10.76 Cl7.24 Mn3 N6'
_chemical_formula_weight         1888.44
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-11-28
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-11-28 deposited with the CCDC.	2022-12-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.648(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   23.5235(8)
_cell_length_b                   9.3471(3)
_cell_length_c                   15.7733(5)
_cell_measurement_reflns_used    9028
_cell_measurement_temperature    282(3)
_cell_measurement_theta_max      26.2050
_cell_measurement_theta_min      2.1670
_cell_volume                     3466.7(2)
_computing_cell_refinement       'CrysAlisPro 1.171.42.63a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.63a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.63a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      282(3)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.787
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -17.00  24.00   0.50    4.00    --    5.54 -99.00  60.00   82
  2  \w     -5.00  21.00   0.50    4.00    --    5.54 -54.00  -0.00   52
  3  \w     12.00  38.00   0.50    4.00    --    5.54 -99.00 -30.00   52
  4  \w    -16.00  30.00   0.50    4.00    --    5.54 -99.00 -90.00   92
  5  \w    -67.00 -21.00   0.50    4.00    --    5.54 -54.00  -0.00   92
  6  \w     -3.00  79.00   0.50    4.00    --    5.54  54.00 143.00  164
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0282285000
_diffrn_orient_matrix_UB_12      -0.0155149000
_diffrn_orient_matrix_UB_13      0.0141113000
_diffrn_orient_matrix_UB_21      0.0031523000
_diffrn_orient_matrix_UB_22      -0.0466492000
_diffrn_orient_matrix_UB_23      -0.0350120000
_diffrn_orient_matrix_UB_31      0.0101424000
_diffrn_orient_matrix_UB_32      0.0577997000
_diffrn_orient_matrix_UB_33      -0.0244919000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_av_unetI/netI     0.0398
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.787
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            30864
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.787
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.769
_diffrn_reflns_theta_min         2.179
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    7.047
_exptl_absorpt_correction_T_max  0.932
_exptl_absorpt_correction_T_min  0.919
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.63a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.809
_exptl_crystal_description       block
_exptl_crystal_F_000             1845
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.031
_refine_diff_density_min         -1.014
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         8547
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0870
_refine_ls_R_factor_gt           0.0410
_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^)+(0.0377P)^2^+3.3537P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0856
_refine_ls_wR_factor_ref         0.0979
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5315
_reflns_number_total             8547
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj04939b2.cif
_cod_data_source_block           xr_2_2_284k_auto
_cod_depositor_comments
'Adding full bibliography for 7062174--7062175.cif.'
_cod_database_code               7062174
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C1 H1 N1 Br1 Cl1 Mn1'
_olex2_refinement_description
;
1. Shared sites
{Cl2, Br2}
{Cl1, Br1}
{Cl3, Br3}
{Cl4, Br4}
{Cl5, Br5}
{Cl6, Br6}
2. Uiso/Uaniso restraints and constraints
Uanis(Cl2) = Uanis(Br2)
Uanis(Cl1) = Uanis(Br1)
Uanis(Cl3) = Uanis(Br3)
Uanis(Cl4) = Uanis(Br4)
Uanis(Cl5) = Uanis(Br5)
Uanis(Cl6) = Uanis(Br6)
3. Others
 Sof(Br2)=1-FVAR(1)
 Sof(Cl2)=FVAR(1)
 Sof(Br1)=1-FVAR(2)
 Sof(Cl1)=FVAR(2)
 Sof(Br3)=1-FVAR(3)
 Sof(Cl3)=FVAR(3)
 Sof(Br4)=1-FVAR(4)
 Sof(Cl4)=FVAR(4)
 Sof(Br5)=1-FVAR(5)
 Sof(Cl5)=FVAR(5)
 Sof(Br6)=1-FVAR(6)
 Sof(Cl6)=FVAR(6)
4.a Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C11(H11A,H11B), C10(H10A,H10B), C4(H4A,H4B), C12(H12A,H12B),
 C17(H17A,H17B), C18(H18A,H18B), C5(H5A,H5B), C6(H6A,H6B)
4.b Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C3(H3A,H3B,
 H3C), C9(H9A,H9B,H9C), C2(H2A,H2B,H2C), C1(H1A,H1B,H1C), C7(H7A,H7B,H7C),
 C8(H8A,H8B,H8C)
;
_shelx_res_checksum              34318
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.933
_oxdiff_exptl_absorpt_empirical_full_min 0.633