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#$Date: 2020-03-28 01:43:14 +0200 (Sat, 28 Mar 2020) $
#$Revision: 249792 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/45/4134571.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_4134571
loop_
_publ_author_name
'Liu, Chun-Yu'
'Chen, Xu-Ran'
'Chen, Hui-Xian'
'Niu, Zheng'
'Hirao, Hajime'
'Braunstein, Pierre'
'Lang, Jian-Ping'
_publ_section_title
;
 Ultrafast Luminescent Light-Up Guest Detection Based on the Lock of the
 Host Molecular Vibration.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c00368
_journal_year                    2020
_chemical_formula_moiety         'C31.33 H28 Cu4 I4 N6 O0.67 P2'
_chemical_formula_sum            'C31.33 H28 Cu4 I4 N6 O0.67 P2'
_chemical_formula_weight         1322.96
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            9
_cell_length_a                   30.0438(12)
_cell_length_b                   30.0438(12)
_cell_length_c                   11.4013(5)
_cell_measurement_reflns_used    9991
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.64
_cell_measurement_theta_min      2.35
_cell_volume                     8912.4(6)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1185
_diffrn_reflns_av_unetI/netI     0.0479
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            65236
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         1.950
_exptl_absorpt_coefficient_mu    5.350
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4777
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 - Bruker AXS area detector scaling and absorption correction'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.218
_exptl_crystal_description       block
_exptl_crystal_F_000             5592
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         6.340
_refine_diff_density_min         -4.785
_refine_diff_density_rms         0.552
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         4545
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.1423
_refine_ls_R_factor_gt           0.1032
_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)+(0.1670P)²+1948.5852P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2967
_refine_ls_wR_factor_ref         0.3437
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3332
_reflns_number_total             4545
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja0c00368_si_002.cif
_cod_data_source_block           1-C2H5OH
_cod_original_cell_volume        8912.4(8)
_cod_database_code               4134571
_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.
;
_shelx_estimated_absorpt_t_min   0.617
_shelx_estimated_absorpt_t_max   0.617
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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
I1 I 0.49035(5) 0.44434(5) 0.89610(12) 0.0346(4) Uani 1 1 d . . . . .
I2 I 0.56657(6) 0.70771(5) 0.39414(12) 0.0382(4) Uani 1 1 d . . . . .
Cu1 Cu 0.46920(7) 0.51406(7) 0.90996(15) 0.0131(4) Uani 1 1 d . . . . .
Cu2 Cu 0.53905(7) 0.65642(7) 0.56575(15) 0.0131(4) Uani 1 1 d . . . . .
P1 P 0.49730(13) 0.57094(13) 0.7669(3) 0.0087(7) Uani 1 1 d . . . . .
N1 N 0.4919(5) 0.5799(5) 0.5289(10) 0.012(2) Uani 1 1 d . . . . .
N2 N 0.4931(5) 0.6575(5) 0.6976(11) 0.013(2) Uani 1 1 d . . . . .
N3 N 0.5887(4) 0.6458(4) 0.6720(10) 0.009(2) Uani 1 1 d . . . . .
C1 C 0.4738(5) 0.5463(5) 0.6188(12) 0.0107(17) Uani 1 1 d . U . . .
C2 C 0.4388(5) 0.4943(5) 0.6041(13) 0.011(3) Uani 1 1 d . . . . .
H2 H 0.4277 0.4714 0.6691 0.014 Uiso 1 1 calc R U . . .
C3 C 0.4208(6) 0.4769(6) 0.4933(14) 0.020(3) Uani 1 1 d . . . . .
H3 H 0.3968 0.4416 0.4801 0.023 Uiso 1 1 calc R U . . .
C4 C 0.4381(7) 0.5119(6) 0.3997(14) 0.022(3) Uani 1 1 d . . . . .
H4 H 0.4252 0.5006 0.3228 0.026 Uiso 1 1 calc R U . . .
C5 C 0.4736(6) 0.5625(6) 0.4196(13) 0.017(3) Uani 1 1 d . . . . .
H5 H 0.4856 0.5858 0.3555 0.020 Uiso 1 1 calc R U . . .
C6 C 0.4822(5) 0.6236(6) 0.7858(13) 0.013(3) Uani 1 1 d . . . . .
C7 C 0.4607(7) 0.6256(7) 0.8882(15) 0.022(3) Uani 1 1 d . . . . .
H7 H 0.4542 0.6011 0.9482 0.026 Uiso 1 1 calc R U . . .
C8 C 0.4483(9) 0.6642(8) 0.9043(17) 0.034(4) Uani 1 1 d . . . . .
H8 H 0.4337 0.6670 0.9757 0.041 Uiso 1 1 calc R U . . .
C9 C 0.4579(7) 0.6979(7) 0.8137(17) 0.029(4) Uani 1 1 d . . . . .
H9 H 0.4490 0.7240 0.8215 0.034 Uiso 1 1 calc R U . . .
C10 C 0.4800(6) 0.6941(6) 0.7124(15) 0.020(3) Uani 1 1 d . . . . .
H10 H 0.4865 0.7178 0.6508 0.024 Uiso 1 1 calc R U . . .
C11 C 0.5665(5) 0.6044(5) 0.7441(11) 0.0057(16) Uani 1 1 d . U . . .
C12 C 0.5959(6) 0.5849(6) 0.7988(12) 0.013(3) Uani 1 1 d . . . . .
H12 H 0.5800 0.5564 0.8509 0.016 Uiso 1 1 calc R U . . .
C13 C 0.6468(6) 0.6075(6) 0.7757(13) 0.016(3) Uani 1 1 d . . . . .
H13 H 0.6666 0.5938 0.8074 0.020 Uiso 1 1 calc R U . . .
C14 C 0.6698(5) 0.6512(6) 0.7047(13) 0.015(3) Uani 1 1 d . . . . .
H14 H 0.7058 0.6684 0.6910 0.017 Uiso 1 1 calc R U . . .
C15 C 0.6407(6) 0.6693(6) 0.6551(13) 0.015(3) Uani 1 1 d . . . . .
H15 H 0.6570 0.6991 0.6072 0.019 Uiso 1 1 calc R U . . .
O1 O 0.360(4) 0.664(5) 0.277(9) 0.11(2) Uiso 0.3333 1 d D U P A -1
H1 H 0.3817 0.6827 0.3285 0.171 Uiso 0.3333 1 calc R U P A -1
C16 C 0.432(4) 0.651(6) 0.249(13) 0.11(2) Uiso 0.3333 1 d D U P A -1
H16A H 0.4485 0.6383 0.1938 0.170 Uiso 0.3333 1 calc R U P A -1
H16B H 0.4564 0.6874 0.2660 0.170 Uiso 0.3333 1 calc R U P A -1
H16C H 0.4239 0.6311 0.3217 0.170 Uiso 0.3333 1 calc R U P A -1
C17 C 0.384(5) 0.646(6) 0.195(9) 0.11(2) Uiso 0.3333 1 d D U P A -1
H17A H 0.3927 0.6653 0.1214 0.136 Uiso 0.3333 1 calc R U P A -1
H17B H 0.3602 0.6089 0.1772 0.136 Uiso 0.3333 1 calc R U P A -1
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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'
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
Cu1 I1 Cu1 77.87(7) . 10_667 ?
Cu2 I2 Cu1 116.61(8) . 15_556 ?
P1 Cu1 I1 116.58(12) . . ?
P1 Cu1 I2 111.79(12) . 14_456 ?
I1 Cu1 I2 108.61(8) . 14_456 ?
P1 Cu1 I1 111.14(12) . 10_667 ?
I1 Cu1 I1 102.13(7) . 10_667 ?
I2 Cu1 I1 105.66(8) 14_456 10_667 ?
N1 Cu2 N2 94.3(5) . . ?
N1 Cu2 N3 95.4(5) . . ?
N2 Cu2 N3 96.7(5) . . ?
N1 Cu2 I2 112.3(3) . . ?
N2 Cu2 I2 127.8(4) . . ?
N3 Cu2 I2 122.7(3) . . ?
C11 P1 C1 101.2(6) . . ?
C11 P1 C6 104.1(6) . . ?
C1 P1 C6 103.9(6) . . ?
C11 P1 Cu1 115.0(4) . . ?
C1 P1 Cu1 116.6(5) . . ?
C6 P1 Cu1 114.3(5) . . ?
C1 N1 C5 118.4(12) . . ?
C1 N1 Cu2 118.5(9) . . ?
C5 N1 Cu2 122.7(10) . . ?
C10 N2 C6 117.5(13) . . ?
C10 N2 Cu2 125.2(11) . . ?
C6 N2 Cu2 116.4(10) . . ?
C11 N3 C15 117.9(12) . . ?
C11 N3 Cu2 115.9(9) . . ?
C15 N3 Cu2 124.4(10) . . ?
N1 C1 C2 123.0(13) . . ?
N1 C1 P1 117.9(10) . . ?
C2 C1 P1 119.1(11) . . ?
C3 C2 C1 118.2(13) . . ?
C3 C2 H2 120.9 . . ?
C1 C2 H2 120.9 . . ?
C2 C3 C4 119.2(14) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 H3 120.4 . . ?
C5 C4 C3 119.8(15) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
N1 C5 C4 121.4(14) . . ?
N1 C5 H5 119.3 . . ?
C4 C5 H5 119.3 . . ?
C7 C6 N2 123.6(15) . . ?
C7 C6 P1 117.5(12) . . ?
N2 C6 P1 118.9(11) . . ?
C6 C7 C8 118.8(16) . . ?
C6 C7 H7 120.6 . . ?
C8 C7 H7 120.6 . . ?
C9 C8 C7 118.0(17) . . ?
C9 C8 H8 121.0 . . ?
C7 C8 H8 121.0 . . ?
C10 C9 C8 120.3(17) . . ?
C10 C9 H9 119.9 . . ?
C8 C9 H9 119.9 . . ?
N2 C10 C9 121.8(16) . . ?
N2 C10 H10 119.1 . . ?
C9 C10 H10 119.1 . . ?
N3 C11 C12 121.5(12) . . ?
N3 C11 P1 119.6(9) . . ?
C12 C11 P1 118.9(10) . . ?
C13 C12 C11 118.9(14) . . ?
C13 C12 H12 120.5 . . ?
C11 C12 H12 120.5 . . ?
C12 C13 C14 119.4(14) . . ?
C12 C13 H13 120.3 . . ?
C14 C13 H13 120.3 . . ?
C15 C14 C13 120.1(13) . . ?
C15 C14 H14 120.0 . . ?
C13 C14 H14 120.0 . . ?
C14 C15 N3 122.1(14) . . ?
C14 C15 H15 119.0 . . ?
N3 C15 H15 119.0 . . ?
C17 O1 H1 109.5 . . ?
C17 C16 H16A 109.5 . . ?
C17 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C17 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O1 C17 C16 110(3) . . ?
O1 C17 H17A 109.7 . . ?
C16 C17 H17A 109.7 . . ?
O1 C17 H17B 109.7 . . ?
C16 C17 H17B 109.7 . . ?
H17A C17 H17B 108.2 . . ?
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
I1 Cu1 2.479(2) . ?
I1 Cu1 2.532(2) 10_667 ?
I2 Cu2 2.369(2) . ?
I2 Cu1 2.501(2) 15_556 ?
Cu1 P1 2.203(4) . ?
Cu1 I2 2.501(2) 14_456 ?
Cu1 I1 2.532(2) 10_667 ?
Cu2 N1 2.052(12) . ?
Cu2 N2 2.052(13) . ?
Cu2 N3 2.066(12) . ?
P1 C11 1.821(13) . ?
P1 C1 1.836(14) . ?
P1 C6 1.864(16) . ?
N1 C1 1.348(18) . ?
N1 C5 1.357(18) . ?
N2 C10 1.35(2) . ?
N2 C6 1.349(19) . ?
N3 C11 1.356(16) . ?
N3 C15 1.370(18) . ?
C1 C2 1.390(19) . ?
C2 C3 1.37(2) . ?
C2 H2 0.9500 . ?
C3 C4 1.40(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.37(2) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C6 C7 1.35(2) . ?
C7 C8 1.40(2) . ?
C7 H7 0.9500 . ?
C8 C9 1.37(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.37(2) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C11 C12 1.424(19) . ?
C12 C13 1.35(2) . ?
C12 H12 0.9500 . ?
C13 C14 1.40(2) . ?
C13 H13 0.9500 . ?
C14 C15 1.36(2) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
O1 C17 1.46(2) . ?
O1 H1 0.8400 . ?
C16 C17 1.50(2) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 N1 C1 C2 3(2) . . . . ?
Cu2 N1 C1 C2 175.2(11) . . . . ?
C5 N1 C1 P1 -177.9(11) . . . . ?
Cu2 N1 C1 P1 -5.4(15) . . . . ?
C11 P1 C1 N1 -51.9(12) . . . . ?
C6 P1 C1 N1 55.9(12) . . . . ?
Cu1 P1 C1 N1 -177.4(9) . . . . ?
C11 P1 C1 C2 127.5(11) . . . . ?
C6 P1 C1 C2 -124.7(11) . . . . ?
Cu1 P1 C1 C2 2.0(13) . . . . ?
N1 C1 C2 C3 -2(2) . . . . ?
P1 C1 C2 C3 178.4(12) . . . . ?
C1 C2 C3 C4 0(2) . . . . ?
C2 C3 C4 C5 2(3) . . . . ?
C1 N1 C5 C4 -1(2) . . . . ?
Cu2 N1 C5 C4 -173.1(13) . . . . ?
C3 C4 C5 N1 -1(3) . . . . ?
C10 N2 C6 C7 -2(2) . . . . ?
Cu2 N2 C6 C7 167.5(13) . . . . ?
C10 N2 C6 P1 177.8(11) . . . . ?
Cu2 N2 C6 P1 -12.6(14) . . . . ?
C11 P1 C6 C7 -119.7(13) . . . . ?
C1 P1 C6 C7 134.7(13) . . . . ?
Cu1 P1 C6 C7 6.6(14) . . . . ?
C11 P1 C6 N2 60.4(12) . . . . ?
C1 P1 C6 N2 -45.2(12) . . . . ?
Cu1 P1 C6 N2 -173.3(9) . . . . ?
N2 C6 C7 C8 1(3) . . . . ?
P1 C6 C7 C8 -179.1(15) . . . . ?
C6 C7 C8 C9 1(3) . . . . ?
C7 C8 C9 C10 -2(3) . . . . ?
C6 N2 C10 C9 2(2) . . . . ?
Cu2 N2 C10 C9 -167.0(13) . . . . ?
C8 C9 C10 N2 0(3) . . . . ?
C15 N3 C11 C12 -1.3(19) . . . . ?
Cu2 N3 C11 C12 163.6(10) . . . . ?
C15 N3 C11 P1 -178.7(10) . . . . ?
Cu2 N3 C11 P1 -13.7(13) . . . . ?
C1 P1 C11 N3 64.3(11) . . . . ?
C6 P1 C11 N3 -43.3(12) . . . . ?
Cu1 P1 C11 N3 -169.1(9) . . . . ?
C1 P1 C11 C12 -113.1(11) . . . . ?
C6 P1 C11 C12 139.3(11) . . . . ?
Cu1 P1 C11 C12 13.5(12) . . . . ?
N3 C11 C12 C13 -2(2) . . . . ?
P1 C11 C12 C13 175.5(11) . . . . ?
C11 C12 C13 C14 4(2) . . . . ?
C12 C13 C14 C15 -3(2) . . . . ?
C13 C14 C15 N3 0(2) . . . . ?
C11 N3 C15 C14 2(2) . . . . ?
Cu2 N3 C15 C14 -161.3(11) . . . . ?
