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_7062175
_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
'Br1.101 Cl2.899 Mn, 6(C6 H15 Br N), 2(Br1.921 Cl2.079 Mn)'
_chemical_formula_sum            'C36 H90 Br10.94 Cl7.06 Mn3 N6'
_chemical_formula_weight         1896.45
_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   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-11-26
_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                 91.605(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   23.6709(12)
_cell_length_b                   9.4002(4)
_cell_length_c                   15.9372(7)
_cell_measurement_reflns_used    6704
_cell_measurement_temperature    374.98(10)
_cell_measurement_theta_max      25.9840
_cell_measurement_theta_min      2.1610
_cell_volume                     3544.8(3)
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      374.98(10)
_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 0.812
_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     18.00  60.00   0.50    4.00    --   -5.65  53.00 143.00   84
  2  \w    -78.00   4.00   0.50    4.00    --   -5.65 -53.00  -0.00  164
  3  \w    -10.00  37.00   0.50    4.00    --    4.87 -99.00  90.00   94
  4  \w     -3.00  37.00   0.50    4.00    --    4.87 -99.00 -30.00   80
  5  \w    -17.00   8.00   0.50    4.00    --    4.87 -99.00 -90.00   50
  6  \w    -17.00  37.00   0.50    4.00    --    4.87 -99.00-150.00  108
;
_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      -0.0281767000
_diffrn_orient_matrix_UB_12      -0.0149134000
_diffrn_orient_matrix_UB_13      -0.0135758000
_diffrn_orient_matrix_UB_21      -0.0030839000
_diffrn_orient_matrix_UB_22      -0.0461587000
_diffrn_orient_matrix_UB_23      0.0347615000
_diffrn_orient_matrix_UB_31      -0.0097672000
_diffrn_orient_matrix_UB_32      0.0577980000
_diffrn_orient_matrix_UB_33      0.0242739000
_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  0.0493
_diffrn_reflns_av_unetI/netI     0.0638
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.812
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            35465
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.812
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.839
_diffrn_reflns_theta_min         1.721
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.987
_exptl_absorpt_correction_T_max  0.933
_exptl_absorpt_correction_T_min  0.920
_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    1.777
_exptl_crystal_description       block
_exptl_crystal_F_000             1852
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.343
_refine_diff_density_min         -0.707
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         9063
_refine_ls_number_restraints     374
_refine_ls_restrained_S_all      1.247
_refine_ls_R_factor_all          0.1551
_refine_ls_R_factor_gt           0.0562
_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^)+(0.0782P)^2^+2.5110P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1443
_refine_ls_wR_factor_ref         0.1791
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3956
_reflns_number_total             9063
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj04939b2.cif
_cod_data_source_block           xr_2_2_375k_auto
_cod_depositor_comments
'Adding full bibliography for 7062174--7062175.cif.'
_cod_database_code               7062175
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{Cl5, Br5}
{Cl3, Br3}
{Cl4, Br4}
{Cl6, Br6}
{Cl2, Br2}
{Cl1, Br1}
3. Restrained distances
 N1-C1 = N4-C17 = N4-C15 = N4-C19 = N4-C21
 1.47 with sigma of 0.01
 C24-C23 = C23-C21
 1.54 with sigma of 0.01
 Br10-C24
 1.95 with sigma of 0.01
 C15-C17
 2.55 with sigma of 0.02
 C17-C21
 2.5 with sigma of 0.02
 C17-C19
 2.55 with sigma of 0.02
 C19-C21
 2.5 with sigma of 0.02
 N4-C15 \\sim N3-C14 \\sim N4-C19 \\sim N3-C18 \\sim N4-C17 \\sim N3-C16 \\sim
N4-C21 \\sim N3-C20 \\sim C21-
 C23 \\sim C20-C22 \\sim C23-C24 \\sim C22-C25 \\sim Br10-C24 \\sim Br8-C25
 with sigma of 0.02
 N1-C3 \\sim N1-C4
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C23 \\sim Br10 \\sim C24 \\sim C21 \\sim N4 \\sim C15 \\sim C19 \\sim C17 \\sim
C20 \\sim C14 \\sim N3 \\sim C18 \\sim C16 \\sim C22 \\sim C25 \\sim Br8:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C1 \\sim Br9 \\sim C7 \\sim C6 \\sim C5 \\sim N1 \\sim C4 \\sim C3 \\sim C2:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(Cl5) = Uanis(Br5)
Uanis(Cl2) = Uanis(Br2)
Uanis(Cl6) = Uanis(Br6)
Uanis(Cl3) = Uanis(Br3)
Uanis(Cl1) = Uanis(Br1)
Uanis(Cl4) = Uanis(Br4)
5. Others
 Sof(Br1)=1-FVAR(1)
 Sof(Cl1)=FVAR(1)
 Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=1-FVAR(2)
 Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=FVAR(2)
 Sof(Br10)=Sof(N4)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(C21)=Sof(H21A)=
 Sof(H21B)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=Sof(C17)=Sof(H17A)=Sof(H17B)=
 Sof(H17C)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(C24)=Sof(H24A)=Sof(H24B)=1-FVAR(3)
 Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(Br8)=Sof(C25)=Sof(H25A)=Sof(H25B)=
 Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(N3)=Sof(C18)=
 Sof(H18A)=Sof(H18B)=Sof(H18C)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=FVAR(3)
 Sof(Br2)=1-FVAR(4)
 Sof(Cl2)=FVAR(4)
 Sof(Br4)=1-FVAR(5)
 Sof(Cl4)=FVAR(5)
 Sof(Br5)=1-FVAR(6)
 Sof(Cl5)=FVAR(6)
 Sof(Br6)=1-FVAR(7)
 Sof(Cl6)=FVAR(7)
 Sof(Br3)=1-FVAR(8)
 Sof(Cl3)=FVAR(8)
6.a Riding coordinates:
 C15(H15A,H15B,H15C), C17(H17A,H17B,H17C)
6.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C11(H11A,H11B), C6(H6A,H6B), C12(H12A,H12B), C13(H13A,H13B),
 C7(H7A,H7B), C21(H21A,H21B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B),
 C22(H22A,H22B), C20(H20A,H20B)
6.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C2(H2A,H2B,H2C),
 C19(H19A,H19B,H19C), C1(H1A,H1B,H1C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C),
 C14(H14A,H14B,H14C), C18(H18A,H18B,H18C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              24635
_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 2.120
_oxdiff_exptl_absorpt_empirical_full_min 0.634