Guest-Induced Reversible Phase Transformation of Organic–Inorganic Phenylpiperazinium Antimony (III) Chlorides with Solvatochromic Photoluminescence
Li, Xianli; Peng, Chao; Xiao, Yonghong; Xue, Dongfeng; Luo, Binbin; Huang, Xiao-Chun; The Journal of Physical Chemistry C 125 (2021) 25112–25118; doi:10.1021/acs.jpcc.1c07725

data_1565532
_publ_section_title
;
 Guest-Induced Reversible Phase Transformation of Organic--Inorganic
 Phenylpiperazinium Antimony (III) Chlorides with Solvatochromic
 Photoluminescence
;
_journal_issue                   45
_journal_name_full               'The Journal of Physical Chemistry C'
_journal_page_first              25112
_journal_page_last               25118
_journal_paper_doi               10.1021/acs.jpcc.1c07725
_journal_volume                  125
_journal_year                    2021
_chemical_formula_moiety         'Cl4 Sb, 3(Cl), 2(C10 H16 N2), 2(H2 O)'
_chemical_formula_sum            'C20 H36 Cl7 N4 O2 Sb'
_chemical_formula_weight         734.43
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-08-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 101.837(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.8872(3)
_cell_length_b                   27.0504(5)
_cell_length_c                   8.1864(2)
_cell_measurement_reflns_used    5774
_cell_measurement_temperature    298.86(10)
_cell_measurement_theta_max      65.1950
_cell_measurement_theta_min      6.4070
_cell_volume                     3443.33(13)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      298.86(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.924
_diffrn_measured_fraction_theta_max 0.975
_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     -2.00  23.00   0.50    0.61    --    0.00  38.00 -60.00   50
  2  \w     31.00  81.00   0.50    0.61    --    0.00  38.00 -60.00  100
  3  \w    -67.00 -41.00   0.50    0.61    --    0.00 -38.00  60.00   52
  4  \w     63.00  88.00   0.50    0.61    --    0.00  77.00  60.00   50
  5  \w     -2.00  24.00   0.50    2.44    --   77.80 -30.00  30.00   52
  6  \w     36.00  87.00   0.50    2.44    --   77.80 -30.00  30.00  102
  7  \w     49.00 165.00   0.50    2.44    --   77.80  82.00  30.00  232
  8  \w     12.00  38.00   0.50    2.44    --   77.80 -61.00 -60.00   52
  9  \w     68.00  93.00   0.50    2.44    --   77.80 -82.00-120.00   50
 10  \w     28.00  67.00   0.50    2.44    --   77.80 -82.00-120.00   78
 11  \w     66.00  95.00   0.50    2.44    --   77.80 -61.00 -60.00   58
 12  \w     32.00 107.00   0.50    2.44    --   77.80 -82.00 -90.00  150
 13  \w     21.00  96.00   0.50    2.44    --   77.80 -61.00 -90.00  150
 14  \w      1.00  89.00   0.50    2.44    --   77.80 -15.00  30.00  176
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0421464000
_diffrn_orient_matrix_UB_12      -0.0407906000
_diffrn_orient_matrix_UB_13      -0.0872259000
_diffrn_orient_matrix_UB_21      0.0288679000
_diffrn_orient_matrix_UB_22      0.0391307000
_diffrn_orient_matrix_UB_23      -0.1138247000
_diffrn_orient_matrix_UB_31      0.0849218000
_diffrn_orient_matrix_UB_32      0.0069204000
_diffrn_orient_matrix_UB_33      0.1280441000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_unetI/netI     0.0301
_diffrn_reflns_Laue_measured_fraction_full 0.924
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            8607
_diffrn_reflns_point_group_measured_fraction_full 0.924
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         65.261
_diffrn_reflns_theta_min         3.268
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.536
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54563
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_description       block
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.524
_refine_diff_density_min         -0.630
_refine_diff_density_rms         0.067
_refine_ls_extinction_coef       0.00013(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     159
_refine_ls_number_reflns         2883
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_gt           0.0294
_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^)+(0.0505P)^2^+1.6628P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0828
_refine_ls_wR_factor_ref         0.0836
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2701
_reflns_number_total             2883
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jp1c07725_si_002.cif
_cod_data_source_block           (PhPi)2SbCl7-xH2O
_cod_database_code               1565532
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C H N O Sb Cl'
_chemical_oxdiff_usercomment     'C H N O Sb Cl'
_shelx_estimated_absorpt_t_max   0.596
_shelx_estimated_absorpt_t_min   0.392
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     61.08
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O1(H1C,H1D)
2.b Ternary CH refined with riding coordinates:
 N1(H1)
2.c Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), C2(H2C,H2D), C4(H4A,H4B), C3(H3A,H3B), C1(H1A,H1B)
2.d Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C10(H10), C9(H9)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              68602
_shelx_hkl_checksum              46297
_shelx_fab_checksum              11825
_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 1.840
_oxdiff_exptl_absorpt_empirical_full_min 0.639