#------------------------------------------------------------------------------
#$Date: 2021-03-05 04:00:24 +0200 (Fri, 05 Mar 2021) $
#$Revision: 262628 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/62/7706221.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_7706221
loop_
_publ_author_name
'Zhan, Shun-Ze'
'Chen, Wei'
'Zheng, Ji'
'Ng, Seik Weng'
'Li, Dan'
_publ_section_title
;
 Luminescent polymorphic aggregates of trinuclear Cu(I)-pyrazolate tuned
 by intertrimeric CuNPy weak coordination bonds.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1733
_journal_page_last               1739
_journal_paper_doi               10.1039/d0dt03661g
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'Cu3 (C10 H10 N3 S)3, (C2 H6 O)'
_chemical_formula_sum            'C32 H36 Cu3 N9 O S3'
_chemical_formula_weight         849.50
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-12-21 deposited with the CCDC.	2020-12-24 downloaded from the CCDC.
;
_cell_angle_alpha                102.747(2)
_cell_angle_beta                 97.489(2)
_cell_angle_gamma                93.497(2)
_cell_formula_units_Z            2
_cell_length_a                   10.0630(3)
_cell_length_b                   12.0715(3)
_cell_length_c                   14.8898(4)
_cell_measurement_reflns_used    8131
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.4760
_cell_measurement_theta_min      3.7470
_cell_volume                     1741.57(8)
_computing_cell_refinement       'CrysAlisPro 1.171.41.67a (Rigaku OD, 2020)'
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction        'CrysAlisPro 1.171.41.67a (Rigaku OD, 2020)'
_computing_molecular_graphics    OLEX
_computing_publication_material  OLEX
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4098
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_av_unetI/netI     0.0391
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14430
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.576
_diffrn_reflns_theta_min         3.449
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    2.037
_exptl_absorpt_correction_T_max  0.631
_exptl_absorpt_correction_T_min  0.498
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.67a (Rigaku Oxford Diffraction, 2020)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_description       irregular
_exptl_crystal_F_000             868
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.418
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         7725
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0287
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0296P)²+0.5649P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0660
_refine_ls_wR_factor_ref         0.0697
_reflns_number_gt                6619
_reflns_number_total             7725
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt03661g2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7706219--7706223.cif.'
_cod_database_code               7706221
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.429
_shelx_estimated_absorpt_t_max   0.580
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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
Cu1 Cu 0.66547(2) 0.10392(2) 0.60509(2) 0.01564(7) Uani 1 1 d . . . . .
Cu2 Cu 0.39363(3) 0.22140(2) 0.65515(2) 0.01797(7) Uani 1 1 d . . . . .
Cu3 Cu 0.59399(2) 0.13583(2) 0.81582(2) 0.01615(7) Uani 1 1 d . . . . .
S1 S 0.41046(5) 0.20067(4) 0.26995(4) 0.01607(11) Uani 1 1 d . . . . .
S2 S 0.15071(5) 0.30297(4) 0.98686(4) 0.01585(11) Uani 1 1 d . . . . .
S3 S 1.12434(5) -0.01061(4) 0.82244(4) 0.01602(11) Uani 1 1 d . . . . .
N1 N 0.54604(17) 0.13801(14) 0.51102(12) 0.0149(4) Uani 1 1 d . . . . .
N2 N 0.42403(17) 0.17854(14) 0.52963(12) 0.0154(4) Uani 1 1 d . . . . .
N3 N 0.5495(2) 0.58038(16) 0.31671(13) 0.0302(5) Uani 1 1 d . . . . .
N4 N 0.34310(17) 0.21835(14) 0.77259(12) 0.0144(3) Uani 1 1 d . . . . .
N5 N 0.42054(16) 0.17262(13) 0.83636(12) 0.0137(3) Uani 1 1 d . . . . .
N6 N 0.29132(18) 0.68428(15) 1.07909(13) 0.0218(4) Uani 1 1 d . . . . .
N7 N 0.75740(16) 0.08211(13) 0.78559(11) 0.0138(3) Uani 1 1 d . . . . .
N8 N 0.79211(17) 0.07587(14) 0.69795(11) 0.0143(3) Uani 1 1 d . . . . .
N9 N 1.0588(2) -0.39810(17) 0.77412(19) 0.0435(6) Uani 1 1 d . . . . .
C1 C 0.6779(2) 0.09712(19) 0.38068(15) 0.0224(5) Uani 1 1 d . . . . .
H1A H 0.727714 0.053577 0.419942 0.034 Uiso 1 1 calc R U . . .
H1B H 0.735986 0.163537 0.376702 0.034 Uiso 1 1 calc R U . . .
H1C H 0.649666 0.048608 0.318161 0.034 Uiso 1 1 calc R U . . .
C2 C 0.5571(2) 0.13606(16) 0.42204(14) 0.0145(4) Uani 1 1 d . . . . .
C3 C 0.4418(2) 0.17524(16) 0.38175(14) 0.0145(4) Uani 1 1 d . . . . .
C4 C 0.3610(2) 0.20040(16) 0.45203(14) 0.0148(4) Uani 1 1 d . . . . .
C5 C 0.2252(2) 0.24410(19) 0.44736(15) 0.0206(5) Uani 1 1 d . . . . .
H5A H 0.195633 0.254806 0.508595 0.031 Uiso 1 1 calc R U . . .
H5B H 0.160945 0.188978 0.401425 0.031 Uiso 1 1 calc R U . . .
H5C H 0.230022 0.317189 0.428984 0.031 Uiso 1 1 calc R U . . .
C6 C 0.4658(2) 0.34771(17) 0.29070(14) 0.0170(4) Uani 1 1 d . . . . .
C7 C 0.5387(3) 0.4087(2) 0.37383(18) 0.0384(7) Uani 1 1 d . . . . .
H7 H 0.562225 0.372783 0.423625 0.046 Uiso 1 1 calc R U . . .
C8 C 0.5767(3) 0.5231(2) 0.38309(19) 0.0481(8) Uani 1 1 d . . . . .
H8 H 0.625890 0.564035 0.440957 0.058 Uiso 1 1 calc R U . . .
C9 C 0.4803(2) 0.52021(18) 0.23695(15) 0.0222(5) Uani 1 1 d . . . . .
H9 H 0.459525 0.558211 0.188102 0.027 Uiso 1 1 calc R U . . .
C10 C 0.4363(2) 0.40537(18) 0.22054(15) 0.0196(4) Uani 1 1 d . . . . .
H10 H 0.386752 0.366711 0.162121 0.023 Uiso 1 1 calc R U . . .
C11 C 0.1386(2) 0.32147(18) 0.76195(15) 0.0203(5) Uani 1 1 d . . . . .
H11A H 0.164057 0.325243 0.701306 0.030 Uiso 1 1 calc R U . . .
H11B H 0.133031 0.398840 0.798387 0.030 Uiso 1 1 calc R U . . .
H11C H 0.050822 0.277402 0.752747 0.030 Uiso 1 1 calc R U . . .
C12 C 0.24171(19) 0.26505(16) 0.81279(14) 0.0135(4) Uani 1 1 d . . . . .
C13 C 0.25407(19) 0.25153(16) 0.90436(14) 0.0134(4) Uani 1 1 d . . . . .
C14 C 0.36818(19) 0.19207(16) 0.91600(14) 0.0131(4) Uani 1 1 d . . . . .
C15 C 0.4250(2) 0.14701(17) 0.99659(15) 0.0184(4) Uani 1 1 d . . . . .
H15A H 0.523494 0.156142 1.003828 0.028 Uiso 1 1 calc R U . . .
H15B H 0.394041 0.065957 0.985789 0.028 Uiso 1 1 calc R U . . .
H15C H 0.394797 0.189223 1.053291 0.028 Uiso 1 1 calc R U . . .
C16 C 0.2070(2) 0.45008(16) 1.02006(14) 0.0144(4) Uani 1 1 d . . . . .
C17 C 0.1419(2) 0.52270(17) 1.08342(15) 0.0173(4) Uani 1 1 d . . . . .
H17 H 0.067586 0.493980 1.107619 0.021 Uiso 1 1 calc R U . . .
C18 C 0.1877(2) 0.63727(17) 1.11016(15) 0.0201(5) Uani 1 1 d . . . . .
H18 H 0.142806 0.685703 1.153384 0.024 Uiso 1 1 calc R U . . .
C19 C 0.3507(2) 0.61346(17) 1.01756(16) 0.0215(5) Uani 1 1 d . . . . .
H19 H 0.423733 0.644764 0.993712 0.026 Uiso 1 1 calc R U . . .
C20 C 0.3133(2) 0.49812(17) 0.98631(15) 0.0188(4) Uani 1 1 d . . . . .
H20 H 0.359532 0.452256 0.942345 0.023 Uiso 1 1 calc R U . . .
C21 C 0.8550(2) 0.05501(19) 0.93894(15) 0.0206(5) Uani 1 1 d . . . . .
H21A H 0.772868 0.087323 0.957151 0.031 Uiso 1 1 calc R U . . .
H21B H 0.933807 0.100707 0.978410 0.031 Uiso 1 1 calc R U . . .
H21C H 0.854103 -0.023634 0.946508 0.031 Uiso 1 1 calc R U . . .
C22 C 0.8616(2) 0.05595(16) 0.83987(14) 0.0142(4) Uani 1 1 d . . . . .
C23 C 0.96559(19) 0.03089(16) 0.78729(14) 0.0135(4) Uani 1 1 d . . . . .
C24 C 0.9182(2) 0.04512(16) 0.69914(14) 0.0146(4) Uani 1 1 d . . . . .
C25 C 0.9875(2) 0.0325(2) 0.61510(15) 0.0240(5) Uani 1 1 d . . . . .
H25A H 0.924048 0.041806 0.562043 0.036 Uiso 1 1 calc R U . . .
H25B H 1.020014 -0.043365 0.600834 0.036 Uiso 1 1 calc R U . . .
H25C H 1.063818 0.090867 0.627287 0.036 Uiso 1 1 calc R U . . .
C26 C 1.0940(2) -0.15985(16) 0.80373(14) 0.0142(4) Uani 1 1 d . . . . .
C27 C 0.9664(2) -0.21772(18) 0.78607(15) 0.0195(4) Uani 1 1 d . . . . .
H27 H 0.888339 -0.177398 0.783723 0.023 Uiso 1 1 calc R U . . .
C28 C 0.9553(2) -0.3347(2) 0.77203(19) 0.0323(6) Uani 1 1 d . . . . .
H28 H 0.867295 -0.373017 0.759949 0.039 Uiso 1 1 calc R U . . .
C29 C 1.1812(3) -0.3409(2) 0.7928(2) 0.0360(6) Uani 1 1 d . . . . .
H29 H 1.257103 -0.383710 0.795769 0.043 Uiso 1 1 calc R U . . .
C30 C 1.2044(2) -0.22418(19) 0.80810(16) 0.0215(5) Uani 1 1 d . . . . .
H30 H 1.293628 -0.188176 0.821320 0.026 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'
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'
S S 0.1246 0.1234 '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'
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
N1 Cu1 N8 176.74(7) . . ?
N4 Cu2 N2 163.01(7) . . ?
N4 Cu2 N3 97.65(7) . 2_666 ?
N2 Cu2 N3 99.21(7) . 2_666 ?
N5 Cu3 N7 172.93(7) . . ?
C3 S1 C6 101.96(9) . . ?
C13 S2 C16 101.92(9) . . ?
C23 S3 C26 102.92(9) . . ?
C2 N1 N2 108.56(16) . . ?
C2 N1 Cu1 131.06(14) . . ?
N2 N1 Cu1 120.30(13) . . ?
C4 N2 N1 108.06(16) . . ?
C4 N2 Cu2 131.52(14) . . ?
N1 N2 Cu2 118.89(13) . . ?
C9 N3 C8 115.7(2) . . ?
C9 N3 Cu2 122.58(16) . 2_666 ?
C8 N3 Cu2 121.52(16) . 2_666 ?
C12 N4 N5 108.23(16) . . ?
C12 N4 Cu2 129.71(15) . . ?
N5 N4 Cu2 121.80(12) . . ?
C14 N5 N4 108.84(15) . . ?
C14 N5 Cu3 129.15(14) . . ?
N4 N5 Cu3 119.30(12) . . ?
C19 N6 C18 115.96(18) . . ?
C22 N7 N8 108.62(16) . . ?
C22 N7 Cu3 129.98(14) . . ?
N8 N7 Cu3 121.06(13) . . ?
C24 N8 N7 107.89(16) . . ?
C24 N8 Cu1 133.14(14) . . ?
N7 N8 Cu1 118.92(12) . . ?
C28 N9 C29 115.8(2) . . ?
N1 C2 C3 108.57(18) . . ?
N1 C2 C1 121.61(19) . . ?
C3 C2 C1 129.82(19) . . ?
C2 C3 C4 105.75(18) . . ?
C2 C3 S1 127.32(16) . . ?
C4 C3 S1 126.69(16) . . ?
N2 C4 C3 109.06(18) . . ?
N2 C4 C5 122.08(18) . . ?
C3 C4 C5 128.85(19) . . ?
C7 C6 C10 117.6(2) . . ?
C7 C6 S1 123.12(18) . . ?
C10 C6 S1 119.29(16) . . ?
C8 C7 C6 118.6(2) . . ?
N3 C8 C7 124.9(2) . . ?
N3 C9 C10 124.1(2) . . ?
C9 C10 C6 119.1(2) . . ?
N4 C12 C13 108.86(18) . . ?
N4 C12 C11 121.76(18) . . ?
C13 C12 C11 129.37(18) . . ?
C12 C13 C14 105.63(17) . . ?
C12 C13 S2 126.43(16) . . ?
C14 C13 S2 127.91(16) . . ?
N5 C14 C13 108.44(18) . . ?
N5 C14 C15 121.58(18) . . ?
C13 C14 C15 129.86(18) . . ?
C20 C16 C17 117.60(18) . . ?
C20 C16 S2 123.42(15) . . ?
C17 C16 S2 118.97(15) . . ?
C18 C17 C16 118.67(19) . . ?
N6 C18 C17 124.25(19) . . ?
N6 C19 C20 124.5(2) . . ?
C16 C20 C19 118.97(19) . . ?
N7 C22 C23 108.63(18) . . ?
N7 C22 C21 121.45(18) . . ?
C23 C22 C21 129.92(19) . . ?
C24 C23 C22 105.85(18) . . ?
C24 C23 S3 125.87(15) . . ?
C22 C23 S3 128.27(16) . . ?
N8 C24 C23 108.99(17) . . ?
N8 C24 C25 121.56(19) . . ?
C23 C24 C25 129.44(19) . . ?
C27 C26 C30 117.68(19) . . ?
C27 C26 S3 123.94(16) . . ?
C30 C26 S3 118.37(16) . . ?
C28 C27 C26 118.7(2) . . ?
N9 C28 C27 124.8(2) . . ?
N9 C29 C30 124.4(2) . . ?
C29 C30 C26 118.6(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
Cu1 N1 1.8578(18) . ?
Cu1 N8 1.8575(17) . ?
Cu2 N4 1.8909(17) . ?
Cu2 N2 1.8963(17) . ?
Cu2 N3 2.3572(19) 2_666 ?
Cu3 N5 1.8738(16) . ?
Cu3 N7 1.8765(16) . ?
S1 C3 1.751(2) . ?
S1 C6 1.774(2) . ?
S2 C13 1.747(2) . ?
S2 C16 1.771(2) . ?
S3 C23 1.753(2) . ?
S3 C26 1.762(2) . ?
N1 C2 1.339(3) . ?
N1 N2 1.388(2) . ?
N2 C4 1.331(3) . ?
N3 C9 1.329(3) . ?
N3 C8 1.336(3) . ?
N4 C12 1.341(2) . ?
N4 N5 1.380(2) . ?
N5 C14 1.339(2) . ?
N6 C19 1.337(3) . ?
N6 C18 1.339(3) . ?
N7 C22 1.336(3) . ?
N7 N8 1.382(2) . ?
N8 C24 1.343(3) . ?
N9 C28 1.331(3) . ?
N9 C29 1.339(3) . ?
C1 C2 1.489(3) . ?
C2 C3 1.393(3) . ?
C3 C4 1.400(3) . ?
C4 C5 1.493(3) . ?
C6 C7 1.381(3) . ?
C6 C10 1.389(3) . ?
C7 C8 1.382(4) . ?
C9 C10 1.387(3) . ?
C11 C12 1.491(3) . ?
C12 C13 1.399(3) . ?
C13 C14 1.403(3) . ?
C14 C15 1.486(3) . ?
C16 C20 1.387(3) . ?
C16 C17 1.398(3) . ?
C17 C18 1.384(3) . ?
C19 C20 1.379(3) . ?
C21 C22 1.488(3) . ?
C22 C23 1.396(3) . ?
C23 C24 1.388(3) . ?
C24 C25 1.494(3) . ?
C26 C27 1.388(3) . ?
C26 C30 1.397(3) . ?
C27 C28 1.377(3) . ?
C29 C30 1.377(3) . ?
