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#$Date: 2023-08-31 00:59:29 +0300 (Thu, 31 Aug 2023) $
#$Revision: 285911 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/13/20/7132072.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7132072
loop_
_publ_author_name
'Yin, Meijuan'
'Li, Baihan'
'Yi, Zishuo'
'Zhang, Yuchi'
'Xia, Zhiguo'
'Xu, Yan'
_publ_section_title
;
 Crystal-glass phase transition enabling reversible fluorescence switching
 in zero-dimensional antimony halides
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC03752E
_journal_year                    2023
_chemical_formula_sum            'C44 H48 Cl5 P2 Sb'
_chemical_formula_weight         937.76
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc2gqr21
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2023-08-01 deposited with the CCDC.	2023-08-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.287(16)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.0525(12)
_cell_length_b                   16.9015(17)
_cell_length_c                   13.739(2)
_cell_measurement_reflns_used    10469
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.279
_cell_measurement_theta_min      3.142
_cell_volume                     2203.3(5)
_computing_cell_refinement       'APEX2 (Bruker, 2003-2008)'
_computing_data_collection       'APEX2 (Bruker, 2003-2008)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2005)'
_computing_publication_material  'publCIF (Westrip, 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.857
_diffrn_measurement_device_type  'Bruker PHOTON2 CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0227
_diffrn_reflns_av_unetI/netI     0.0468
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.857
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10469
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.857
_diffrn_reflns_theta_full        29.279
_diffrn_reflns_theta_max         29.279
_diffrn_reflns_theta_min         3.142
_exptl_absorpt_coefficient_mu    1.032
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.5782
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2004/1. Bruker AXS Inc., Madison, Wisconsin, USA, 2004
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_description       block
_exptl_crystal_F_000             956
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.540
_refine_diff_density_min         -1.263
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         5152
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0452
_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/[σ²(Fo²)+(0.0310P)²+2.5918P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0851
_refine_ls_wR_factor_ref         0.1003
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3697
_reflns_number_total             5152
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3cc03752e2.cif
_cod_data_source_block           c
_cod_original_cell_volume        2203.2(6)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7132072
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sb Sb 1.0000 0.5000 0.5000 0.05038(12) Uani 1 2 d S . P . .
Cl1 Cl 0.75929(9) 0.45157(5) 0.37487(7) 0.0519(2) Uani 1 1 d . . . . .
Cl2 Cl 0.88450(10) 0.55665(6) 0.62990(8) 0.0603(3) Uani 1 1 d . . . . .
Cl3 Cl 1.02594(18) 0.38159(9) 0.56845(14) 0.0449(4) Uani 0.5 1 d . . P . .
P P 0.47211(9) 0.22046(5) 0.33405(7) 0.0373(2) Uani 1 1 d . . . . .
C1 C 0.3068(3) 0.18589(19) 0.3402(3) 0.0404(8) Uani 1 1 d . . . . .
C2 C 0.2240(4) 0.2372(2) 0.3745(3) 0.0564(10) Uani 1 1 d . . . . .
H2 H 0.2529 0.2892 0.3911 0.068 Uiso 1 1 calc R U . . .
C3 C 0.0992(4) 0.2112(3) 0.3839(4) 0.0711(13) Uani 1 1 d . . . . .
H3 H 0.0440 0.2453 0.4075 0.085 Uiso 1 1 calc R U . . .
C4 C 0.0566(4) 0.1351(3) 0.3586(3) 0.0682(12) Uani 1 1 d . . . . .
H4 H -0.0278 0.1177 0.3653 0.082 Uiso 1 1 calc R U . . .
C5 C 0.1360(4) 0.0837(3) 0.3236(3) 0.0608(11) Uani 1 1 d . . . . .
H5 H 0.1053 0.0321 0.3060 0.073 Uiso 1 1 calc R U . . .
C6 C 0.2618(4) 0.1091(2) 0.3145(3) 0.0500(9) Uani 1 1 d . . . . .
H6 H 0.3164 0.0745 0.2911 0.060 Uiso 1 1 calc R U . . .
C7 C 0.6063(4) 0.2005(2) 0.4547(3) 0.0444(8) Uani 1 1 d . . . . .
C8 C 0.5847(5) 0.1420(3) 0.5179(3) 0.0665(11) Uani 1 1 d . . . . .
H8 H 0.4988 0.1156 0.4990 0.080 Uiso 1 1 calc R U . . .
C9 C 0.6877(6) 0.1224(3) 0.6078(4) 0.0859(15) Uani 1 1 d . . . . .
H9 H 0.6717 0.0829 0.6498 0.103 Uiso 1 1 calc R U . . .
C10 C 0.8122(6) 0.1602(3) 0.6355(4) 0.0861(16) Uani 1 1 d . . . . .
H10 H 0.8826 0.1460 0.6963 0.103 Uiso 1 1 calc R U . . .
C11 C 0.8370(5) 0.2194(3) 0.5754(4) 0.0828(15) Uani 1 1 d . . . . .
H11 H 0.9236 0.2453 0.5956 0.099 Uiso 1 1 calc R U . . .
C12 C 0.7325(4) 0.2408(2) 0.4842(3) 0.0617(11) Uani 1 1 d . . . . .
H12 H 0.7477 0.2816 0.4437 0.074 Uiso 1 1 calc R U . . .
C13 C 0.5163(3) 0.16994(18) 0.2343(2) 0.0361(7) Uani 1 1 d . . . . .
C14 C 0.6568(4) 0.1579(2) 0.2451(3) 0.0493(9) Uani 1 1 d . . . . .
H14 H 0.7272 0.1746 0.3045 0.059 Uiso 1 1 calc R U . . .
C15 C 0.6916(4) 0.1213(2) 0.1680(3) 0.0562(10) Uani 1 1 d . . . . .
H15 H 0.7860 0.1143 0.1748 0.067 Uiso 1 1 calc R U . . .
C16 C 0.5900(4) 0.0950(2) 0.0817(3) 0.0508(9) Uani 1 1 d . . . . .
H16 H 0.6150 0.0689 0.0307 0.061 Uiso 1 1 calc R U . . .
C17 C 0.4511(4) 0.1071(2) 0.0698(3) 0.0493(9) Uani 1 1 d . . . . .
H17 H 0.3817 0.0895 0.0104 0.059 Uiso 1 1 calc R U . . .
C18 C 0.4134(4) 0.1453(2) 0.1456(3) 0.0449(8) Uani 1 1 d . . . . .
H18 H 0.3189 0.1543 0.1368 0.054 Uiso 1 1 calc R U . . .
C19 C 0.4625(4) 0.32470(19) 0.3086(3) 0.0456(8) Uani 1 1 d . . . . .
H19A H 0.4431 0.3516 0.3648 0.055 Uiso 1 1 calc R U . . .
H19B H 0.5539 0.3426 0.3080 0.055 Uiso 1 1 calc R U . . .
C20 C 0.3528(4) 0.3491(2) 0.2087(3) 0.0528(9) Uani 1 1 d . . . . .
H20A H 0.2609 0.3307 0.2077 0.063 Uiso 1 1 calc R U . . .
H20B H 0.3735 0.3246 0.1515 0.063 Uiso 1 1 calc R U . . .
C21 C 0.3493(5) 0.4381(2) 0.1958(3) 0.0667(12) Uani 1 1 d . . . . .
H21A H 0.3361 0.4622 0.2560 0.080 Uiso 1 1 calc R U . . .
H21B H 0.4397 0.4555 0.1927 0.080 Uiso 1 1 calc R U . . .
C22 C 0.2377(7) 0.4665(3) 0.1032(4) 0.109(2) Uani 1 1 d . . . . .
H22A H 0.2418 0.5231 0.1000 0.130 Uiso 1 1 calc R U . . .
H22B H 0.2512 0.4441 0.0429 0.130 Uiso 1 1 calc R U . . .
H22C H 0.1475 0.4507 0.1063 0.130 Uiso 1 1 calc R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl3 Sb Cl3 180.00(9) . 3_766 ?
Cl3 Sb Cl1 87.07(5) . . ?
Cl3 Sb Cl1 92.93(5) 3_766 . ?
Cl3 Sb Cl1 92.93(5) . 3_766 ?
Cl3 Sb Cl1 87.07(5) 3_766 3_766 ?
Cl1 Sb Cl1 180.0 . 3_766 ?
Cl3 Sb Cl2 93.35(5) . . ?
Cl3 Sb Cl2 86.65(5) 3_766 . ?
Cl1 Sb Cl2 92.33(3) . . ?
Cl1 Sb Cl2 87.67(3) 3_766 . ?
Cl3 Sb Cl2 86.66(5) . 3_766 ?
Cl3 Sb Cl2 93.34(5) 3_766 3_766 ?
Cl1 Sb Cl2 87.67(3) . 3_766 ?
Cl1 Sb Cl2 92.33(3) 3_766 3_766 ?
Cl2 Sb Cl2 180.0 . 3_766 ?
C1 P C7 108.82(17) . . ?
C1 P C13 110.43(15) . . ?
C7 P C13 108.51(15) . . ?
C1 P C19 109.82(16) . . ?
C7 P C19 109.94(17) . . ?
C13 P C19 109.30(16) . . ?
C6 C1 C2 119.4(3) . . ?
C6 C1 P 121.7(3) . . ?
C2 C1 P 118.8(3) . . ?
C3 C2 C1 120.0(4) . . ?
C3 C2 H2 120.0 . . ?
C1 C2 H2 120.0 . . ?
C4 C3 C2 119.8(4) . . ?
C4 C3 H3 120.1 . . ?
C2 C3 H3 120.1 . . ?
C5 C4 C3 121.1(4) . . ?
C5 C4 H4 119.5 . . ?
C3 C4 H4 119.5 . . ?
C4 C5 C6 119.5(4) . . ?
C4 C5 H5 120.2 . . ?
C6 C5 H5 120.2 . . ?
C1 C6 C5 120.1(4) . . ?
C1 C6 H6 119.9 . . ?
C5 C6 H6 119.9 . . ?
C12 C7 C8 119.3(4) . . ?
C12 C7 P 121.3(3) . . ?
C8 C7 P 119.4(3) . . ?
C9 C8 C7 120.9(5) . . ?
C9 C8 H8 119.5 . . ?
C7 C8 H8 119.5 . . ?
C10 C9 C8 119.8(5) . . ?
C10 C9 H9 120.1 . . ?
C8 C9 H9 120.1 . . ?
C9 C10 C11 120.9(5) . . ?
C9 C10 H10 119.5 . . ?
C11 C10 H10 119.5 . . ?
C10 C11 C12 119.9(5) . . ?
C10 C11 H11 120.1 . . ?
C12 C11 H11 120.1 . . ?
C7 C12 C11 119.0(4) . . ?
C7 C12 H12 120.5 . . ?
C11 C12 H12 120.5 . . ?
C18 C13 C14 119.4(3) . . ?
C18 C13 P 121.2(3) . . ?
C14 C13 P 119.3(3) . . ?
C15 C14 C13 119.7(3) . . ?
C15 C14 H14 120.1 . . ?
C13 C14 H14 120.1 . . ?
C16 C15 C14 120.8(4) . . ?
C16 C15 H15 119.6 . . ?
C14 C15 H15 119.6 . . ?
C15 C16 C17 120.0(3) . . ?
C15 C16 H16 120.0 . . ?
C17 C16 H16 120.0 . . ?
C16 C17 C18 120.2(3) . . ?
C16 C17 H17 119.9 . . ?
C18 C17 H17 119.9 . . ?
C13 C18 C17 119.8(3) . . ?
C13 C18 H18 120.1 . . ?
C17 C18 H18 120.1 . . ?
C20 C19 P 115.0(2) . . ?
C20 C19 H19A 108.5 . . ?
P C19 H19A 108.5 . . ?
C20 C19 H19B 108.5 . . ?
P C19 H19B 108.5 . . ?
H19A C19 H19B 107.5 . . ?
C19 C20 C21 111.2(3) . . ?
C19 C20 H20A 109.4 . . ?
C21 C20 H20A 109.4 . . ?
C19 C20 H20B 109.4 . . ?
C21 C20 H20B 109.4 . . ?
H20A C20 H20B 108.0 . . ?
C22 C21 C20 114.0(4) . . ?
C22 C21 H21A 108.7 . . ?
C20 C21 H21A 108.7 . . ?
C22 C21 H21B 108.7 . . ?
C20 C21 H21B 108.7 . . ?
H21A C21 H21B 107.6 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sb Cl3 2.1900(16) . ?
Sb Cl3 2.1900(16) 3_766 ?
Sb Cl1 2.5947(10) . ?
Sb Cl1 2.5947(10) 3_766 ?
Sb Cl2 2.6113(10) . ?
Sb Cl2 2.6113(10) 3_766 ?
P C1 1.790(3) . ?
P C7 1.790(4) . ?
P C13 1.791(3) . ?
P C19 1.793(3) . ?
C1 C6 1.381(5) . ?
C1 C2 1.388(5) . ?
C2 C3 1.376(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.364(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.370(6) . ?
C4 H4 0.9300 . ?
C5 C6 1.379(5) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 C12 1.377(5) . ?
C7 C8 1.380(5) . ?
C8 C9 1.366(6) . ?
C8 H8 0.9300 . ?
C9 C10 1.344(7) . ?
C9 H9 0.9300 . ?
C10 C11 1.372(7) . ?
C10 H10 0.9300 . ?
C11 C12 1.391(6) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 C18 1.377(4) . ?
C13 C14 1.386(4) . ?
C14 C15 1.368(5) . ?
C14 H14 0.9300 . ?
C15 C16 1.359(5) . ?
C15 H15 0.9300 . ?
C16 C17 1.366(5) . ?
C16 H16 0.9300 . ?
C17 C18 1.380(5) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
C19 C20 1.507(5) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 C21 1.513(5) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 C22 1.470(6) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
