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_1565533
_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         'Cl6 Sb, 2(C10 H16 N2), Cl'
_chemical_formula_sum            'C20 H32 Cl7 N4 Sb'
_chemical_formula_weight         698.39
_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   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-08-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 103.0480(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.74300(10)
_cell_length_b                   28.0958(3)
_cell_length_c                   8.45780(10)
_cell_measurement_reflns_used    5287
_cell_measurement_temperature    298.3(7)
_cell_measurement_theta_max      64.9340
_cell_measurement_theta_min      3.1150
_cell_volume                     2949.92(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.7e (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      298.3(7)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.881
_diffrn_measured_fraction_theta_max 0.997
_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    -86.00 -57.00   0.50    1.44    --    0.00 -19.00 -60.00   58
  2  \w    -20.00   6.00   0.50    1.44    --    0.00 -38.00  60.00   52
  3  \w    -81.00 -40.00   0.50    1.44    --    0.00 -38.00  60.00   82
  4  \w    -13.00  16.00   0.50    1.44    --    0.00 -19.00 -60.00   58
  5  \w    -12.00  95.00   0.50    5.75    --   77.80 -45.00-150.00  214
  6  \w    -12.00  78.00   0.50    5.75    --   77.80 -30.00-120.00  180
  7  \w      2.00  96.00   0.50    5.75    --   77.80 -45.00  30.00  188
  8  \w     78.00 167.00   0.50    5.75    --   77.80  61.00 150.00  178
  9  \w     67.00 146.00   0.50    5.75    --   77.80  30.00 150.00  158
 10  \w     34.00  64.00   0.50    5.75    --   77.80 -61.00 -30.00   60
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0961966000
_diffrn_orient_matrix_UB_12      0.0091271000
_diffrn_orient_matrix_UB_13      0.1437453000
_diffrn_orient_matrix_UB_21      0.0671094000
_diffrn_orient_matrix_UB_22      -0.0369569000
_diffrn_orient_matrix_UB_23      -0.0688629000
_diffrn_orient_matrix_UB_31      0.0405986000
_diffrn_orient_matrix_UB_32      0.0394614000
_diffrn_orient_matrix_UB_33      -0.0977052000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0173
_diffrn_reflns_av_unetI/netI     0.0202
_diffrn_reflns_Laue_measured_fraction_full 0.881
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            6600
_diffrn_reflns_point_group_measured_fraction_full 0.881
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         62.488
_diffrn_reflns_theta_min         3.146
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.382
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70048
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.7e (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_description       block
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.939
_refine_diff_density_min         -0.785
_refine_diff_density_rms         0.144
_refine_ls_extinction_coef       0.00023(5)
_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   1.257
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         2361
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.237
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0644
_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^)+(0.0354P)^2^+72.7388P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1766
_refine_ls_wR_factor_ref         0.1770
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2278
_reflns_number_total             2361
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jp1c07725_si_003.cif
_cod_data_source_block           (PhPi)2SbCl7-V
_cod_database_code               1565533
_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   0.348
_shelx_estimated_absorpt_t_min   0.175
_reflns_odcompleteness_completeness 99.91
_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,H) groups
2. Rigid body (RIGU) restrains
 C8B, C6B, C5B, C9B, C7B, C10B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C6A, C10A, C9A, C7A, C5A, C8A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Others
 Fixed Sof: H1a(0.5) H1b(0.5) C8B(0.5) H8B(0.5) C9B(0.5) H9B(0.5) C10B(0.5)
 H10B(0.5) C5B(0.5) C6B(0.5) H6B(0.5) C7B(0.5) H7B(0.5) C6A(0.5) H6A(0.5)
 C7A(0.5) H7A(0.5) C8A(0.5) H8A(0.5) C9A(0.5) H9A(0.5) C10A(0.5) H10A(0.5)
 C5A(0.5) Cl4(0.4) Cl4A(0.1)
4.a Ternary CH refined with riding coordinates:
 N1(H1a), N1(H1b)
4.b Secondary CH2 refined with riding coordinates:
 N2(H2a,H2b), C3(H3a,H3b), C4(H4a,H4b), C2(H2c,H2d), C1(H1c,H1d)
4.c Aromatic/amide H refined with riding coordinates:
 C8B(H8B), C9B(H9B), C10B(H10B), C6B(H6B), C7B(H7B), C6A(H6A), C7A(H7A),
 C8A(H8A), C9A(H9A), C10A(H10A)
4.d Fitted hexagon refined as free rotating group:
 C8B(C9B,C10B,C5B,C6B,C7B), C6A(C7A,C8A,C9A,C10A,C5A)
;
_shelx_res_checksum              71546
_shelx_hkl_checksum              94573
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.277
_oxdiff_exptl_absorpt_empirical_full_min 0.816