Tuning phase transition and fluorescence quenching in 0D organic-inorganic hybrid materials by precise organic cation modification.
Chen, Leqi; Zhou, Zining; Yang, Yawen; Ye, Qiong; Dalton transactions (Cambridge, England : 2003) 54 (2025) 5560–5567; doi:10.1039/d5dt00057b

data_7718285
_publ_section_title
;
 Tuning phase transition and fluorescence quenching in 0D
 organic-inorganic hybrid materials by precise organic cation
 modification.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5560
_journal_page_last               5567
_journal_paper_doi               10.1039/d5dt00057b
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         '2(C6 H16 P), Br4 Mn'
_chemical_formula_sum            'C12 H32 Br4 Mn P2'
_chemical_formula_weight         612.89
_space_group_crystal_system      orthorhombic
_space_group_IT_number           73
_space_group_name_Hall           '-I 2b 2c'
_space_group_name_H-M_alt        'I b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2025-02-09
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2025-02-09 deposited with the CCDC.	2025-02-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   19.0177(4)
_cell_length_b                   19.1067(4)
_cell_length_c                   26.7409(7)
_cell_measurement_reflns_used    8504
_cell_measurement_temperature    275(5)
_cell_measurement_theta_max      69.7450
_cell_measurement_theta_min      2.8220
_cell_volume                     9716.7(4)
_computing_cell_refinement       'CrysAlisPro 1.171.43.129a (Rigaku OD, 2024)'
_computing_data_collection       'CrysAlisPro 1.171.43.129a (Rigaku OD, 2024)'
_computing_data_reduction        'CrysAlisPro 1.171.43.129a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      275(5)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.971
_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     11.00  38.00   0.50    0.19    --   60.54 -30.00-150.00   54
  2  \w     11.00  36.00   0.50    0.19    --   60.54 -30.00 -90.00   50
  3  \w     77.00 115.00   0.50    0.19    --   75.18  30.00  30.00   76
  4  \w     12.00  38.00   0.50    0.19    --   60.54 -30.00  90.00   52
  5  \w     11.00  37.00   0.50    0.19    --   60.54 -30.00 120.00   52
  6  \w     69.00 125.00   0.50    0.19    --   75.18  27.00-140.00  112
  7  \w     12.00  37.00   0.50    0.19    --   60.54 -30.00 -60.00   50
  8  \w     35.00  65.00   0.50    0.19    --   60.54 -94.00 -90.00   60
  9  \w     48.00  81.00   0.50    0.19    --   75.18 -94.00 -60.00   66
 10  \w     40.00  84.00   0.50    0.19    --   75.18 -94.00 -30.00   88
 11  \w     36.00  83.00   0.50    0.19    --   75.18 -94.00 120.00   94
 12  \w   -111.00 -55.00   0.50    0.19    --  -60.94 -27.00  57.00  112
 13  \w    -95.00 -61.00   0.50    0.19    --  -75.65-165.00  61.00   68
 14  \w   -123.00 -93.00   0.50    0.19    --  -74.13 -30.00 -90.00   60
 15  \w    -94.00 -64.00   0.50    0.19    --  -60.94 -30.00-180.00   60
 16  \w   -125.00 -76.00   0.50    0.19    --  -75.65 -27.00  57.00   98
 17  \w    -76.00 -35.00   0.50    0.19    --  -75.65  99.00  38.00   82
 18  \w    -85.00 -18.00   0.50    0.19    --  -60.94 116.00 -62.00  134
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0162450000
_diffrn_orient_matrix_UB_12      -0.0243156000
_diffrn_orient_matrix_UB_13      0.0735063000
_diffrn_orient_matrix_UB_21      -0.0135160000
_diffrn_orient_matrix_UB_22      -0.0763360000
_diffrn_orient_matrix_UB_23      -0.0191108000
_diffrn_orient_matrix_UB_31      0.0535924000
_diffrn_orient_matrix_UB_32      -0.0118810000
_diffrn_orient_matrix_UB_33      -0.0271237000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0938
_diffrn_reflns_av_unetI/netI     0.0416
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            25679
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.340
_diffrn_reflns_theta_min         3.305
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.282
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.21236
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.129a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic light gray'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    gray
_exptl_crystal_density_diffrn    1.676
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       octahedral
_exptl_crystal_F_000             4784
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.021
_refine_diff_density_min         -0.532
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         4683
_refine_ls_number_restraints     83
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0756
_refine_ls_R_factor_gt           0.0598
_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^)+(0.1079P)^2^+3.1876P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1576
_refine_ls_wR_factor_ref         0.1700
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3514
_reflns_number_total             4683
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00057b2.cif
_cod_data_source_block           1_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7718284--7718286.cif.'
_cod_database_code               7718285
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C H P Mn Br '
_shelx_estimated_absorpt_t_max   0.350
_shelx_estimated_absorpt_t_min   0.299
_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. Uiso/Uaniso restraints and constraints
P2 \\sim C10 \\sim C11 \\sim C12 \\sim C10A \\sim C11A \\sim C12A: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Mn1 \\sim Mn2 \\sim Br1 \\sim Br2 \\sim Br6 \\sim Br7 \\sim Br4 \\sim Br3 \\sim
Br5 \\sim Br8: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
3. Same fragment restrains
{P2, C10A, C11A, C12A} sigma for 1-2: 0.01, 1-3: 0.01
as in
{P2, C10, C11, C12}
4. Others
 Sof(C10A)=Sof(H10C)=Sof(H10D)=Sof(C11A)=Sof(H11C)=Sof(H11D)=Sof(C12A)=
 Sof(H12D)=Sof(H12E)=Sof(H12F)=1-FVAR(1)
 Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(C12)=Sof(H12A)=
 Sof(H12B)=Sof(H12C)=FVAR(1)
 Fixed Sof: Br1(0.5) Br2(0.5) Mn1(0.5) Br6(0.5) Mn2(0.5) Br7(0.5) Br4(0.5)
 Br3(0.5) Br5(0.5) Br8(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B), C10(H10A,H10B), C11(H11A,H11B), C10A(H10C,H10D),
 C11A(H11C,H11D)
5.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C6(H6A,H6B,H6C), C7(H7A,
 H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C12(H12A,H12B,H12C), C12A(H12D,
 H12E,H12F)
;
_shelx_res_checksum              27387
_shelx_hkl_checksum              45392
_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 3.629
_oxdiff_exptl_absorpt_empirical_full_min 0.398