#------------------------------------------------------------------------------
#$Date: 2021-03-05 04:00:24 +0200 (Fri, 05 Mar 2021) $
#$Revision: 262628 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/62/7706222.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_7706222
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)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                99.756(7)
_cell_angle_beta                 91.267(7)
_cell_angle_gamma                115.760(8)
_cell_formula_units_Z            2
_cell_length_a                   10.7852(9)
_cell_length_b                   11.6669(9)
_cell_length_c                   16.0438(14)
_cell_measurement_reflns_used    2035
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.4060
_cell_measurement_theta_min      3.5060
_cell_volume                     1781.4(3)
_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    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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 0.888
_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  0.0671
_diffrn_reflns_av_unetI/netI     0.1612
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.888
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12469
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.888
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.577
_diffrn_reflns_theta_min         2.931
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.991
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.96008
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.67a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.584
_exptl_crystal_description       plate
_exptl_crystal_F_000             868
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.657
_refine_diff_density_min         -0.682
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     440
_refine_ls_number_reflns         7328
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.1419
_refine_ls_R_factor_gt           0.0700
_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)+(0.0266P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1035
_refine_ls_wR_factor_ref         0.1301
_reflns_number_gt                4243
_reflns_number_total             7328
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt03661g2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7706219--7706223.cif.'
_cod_database_code               7706222
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.692
_shelx_estimated_absorpt_t_max   0.961
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 0.30467(8) 0.28497(8) 0.47103(4) 0.0169(2) Uani 1 1 d . . . . .
Cu2 Cu 0.60870(8) 0.44732(8) 0.41139(4) 0.0170(2) Uani 1 1 d . . . . .
Cu3 Cu 0.33836(8) 0.39061(8) 0.29829(4) 0.0175(2) Uani 1 1 d . . . . .
S1 S 0.71081(18) 0.29194(16) 0.71116(9) 0.0194(4) Uani 1 1 d . . . . .
S2 S 0.7752(2) 0.57483(19) 0.09011(10) 0.0277(4) Uani 1 1 d . . . . .
S3 S -0.23922(19) 0.17006(19) 0.31988(10) 0.0299(5) Uani 1 1 d . . . . .
O1 O 0.9012(7) 0.0261(7) -0.1276(3) 0.062(2) Uani 1 1 d . . . . .
H1 H 0.911652 0.090852 -0.090728 0.092 Uiso 1 1 calc R U . . .
N1 N 0.4671(5) 0.3329(5) 0.5457(3) 0.0140(12) Uani 1 1 d . . . . .
N2 N 0.5935(5) 0.3891(5) 0.5126(3) 0.0144(12) Uani 1 1 d . . . . .
N3 N 0.6772(6) -0.1122(5) 0.6122(3) 0.0204(13) Uani 1 1 d . . . . .
N4 N 0.6251(5) 0.4815(5) 0.3023(3) 0.0147(12) Uani 1 1 d . . . . .
N5 N 0.5057(5) 0.4585(5) 0.2533(3) 0.0184(13) Uani 1 1 d . . . . .
N6 N 0.8248(7) 0.2219(7) -0.0438(3) 0.0364(17) Uani 1 1 d . . . . .
N7 N 0.1644(5) 0.3152(5) 0.3351(3) 0.0159(12) Uani 1 1 d . . . . .
N8 N 0.1428(5) 0.2660(5) 0.4084(3) 0.0140(12) Uani 1 1 d . . . . .
N9 N -0.3757(7) -0.1765(7) 0.0960(4) 0.0475(19) Uani 1 1 d . . . . .
C1 C 0.3700(6) 0.2248(7) 0.6638(3) 0.0183(15) Uani 1 1 d . . . . .
H1A H 0.300709 0.257094 0.658318 0.027 Uiso 1 1 calc R U . . .
H1B H 0.404406 0.242553 0.723930 0.027 Uiso 1 1 calc R U . . .
H1C H 0.327666 0.131034 0.641448 0.027 Uiso 1 1 calc R U . . .
C2 C 0.4856(7) 0.2905(6) 0.6156(3) 0.0149(15) Uani 1 1 d . . . . .
C3 C 0.6262(6) 0.3193(6) 0.6278(3) 0.0121(14) Uani 1 1 d . . . . .
C4 C 0.6887(7) 0.3785(6) 0.5619(3) 0.0149(15) Uani 1 1 d . . . . .
C5 C 0.8348(7) 0.4253(6) 0.5418(4) 0.0201(15) Uani 1 1 d . . . . .
H5A H 0.840028 0.364965 0.493109 0.030 Uiso 1 1 calc R U . . .
H5B H 0.893187 0.430111 0.591244 0.030 Uiso 1 1 calc R U . . .
H5C H 0.867270 0.511704 0.527971 0.030 Uiso 1 1 calc R U . . .
C6 C 0.6950(7) 0.1346(6) 0.6713(3) 0.0165(15) Uani 1 1 d . . . . .
C7 C 0.7893(7) 0.0980(7) 0.7040(4) 0.0214(16) Uani 1 1 d . . . . .
H7 H 0.861006 0.156216 0.747285 0.026 Uiso 1 1 calc R U . . .
C8 C 0.7772(8) -0.0256(7) 0.6722(4) 0.0272(18) Uani 1 1 d . . . . .
H8 H 0.843052 -0.049575 0.694188 0.033 Uiso 1 1 calc R U . . .
C9 C 0.5849(7) -0.0764(7) 0.5839(3) 0.0195(16) Uani 1 1 d . . . . .
H9 H 0.511272 -0.137575 0.542608 0.023 Uiso 1 1 calc R U . . .
C10 C 0.5905(7) 0.0438(6) 0.6110(3) 0.0190(15) Uani 1 1 d . . . . .
H10 H 0.522369 0.064413 0.588219 0.023 Uiso 1 1 calc R U . . .
C11 C 0.8764(7) 0.5625(7) 0.2914(4) 0.0275(18) Uani 1 1 d . . . . .
H11A H 0.912275 0.645926 0.331466 0.041 Uiso 1 1 calc R U . . .
H11B H 0.935057 0.570157 0.244835 0.041 Uiso 1 1 calc R U . . .
H11C H 0.876877 0.495715 0.320999 0.041 Uiso 1 1 calc R U . . .
C12 C 0.7318(7) 0.5253(7) 0.2562(3) 0.0195(16) Uani 1 1 d . . . . .
C13 C 0.6817(7) 0.5285(7) 0.1758(4) 0.0213(16) Uani 1 1 d . . . . .
C14 C 0.5409(7) 0.4861(6) 0.1765(3) 0.0181(15) Uani 1 1 d . . . . .
C15 C 0.4343(7) 0.4709(8) 0.1088(4) 0.0300(18) Uani 1 1 d . . . . .
H15A H 0.427623 0.404479 0.060117 0.045 Uiso 1 1 calc R U . . .
H15B H 0.460958 0.553759 0.090607 0.045 Uiso 1 1 calc R U . . .
H15C H 0.344296 0.444466 0.131365 0.045 Uiso 1 1 calc R U . . .
C16 C 0.7838(7) 0.4327(7) 0.0400(4) 0.0237(17) Uani 1 1 d . . . . .
C17 C 0.7437(7) 0.3202(7) 0.0717(4) 0.0285(18) Uani 1 1 d . . . . .
H17 H 0.700930 0.312415 0.122941 0.034 Uiso 1 1 calc R U . . .
C18 C 0.7661(8) 0.2199(8) 0.0287(4) 0.036(2) Uani 1 1 d . . . . .
H18 H 0.737910 0.143969 0.052100 0.043 Uiso 1 1 calc R U . . .
C19 C 0.8594(8) 0.3300(9) -0.0758(4) 0.035(2) Uani 1 1 d . . . . .
H19 H 0.899029 0.333418 -0.128223 0.042 Uiso 1 1 calc R U . . .
C20 C 0.8414(7) 0.4359(8) -0.0379(4) 0.0298(18) Uani 1 1 d . . . . .
H20 H 0.867294 0.509483 -0.063645 0.036 Uiso 1 1 calc R U . . .
C21 C 0.0314(7) 0.3317(7) 0.2131(4) 0.0275(18) Uani 1 1 d . . . . .
H21A H 0.104877 0.419569 0.215511 0.041 Uiso 1 1 calc R U . . .
H21B H -0.059075 0.330993 0.203712 0.041 Uiso 1 1 calc R U . . .
H21C H 0.041558 0.271519 0.166355 0.041 Uiso 1 1 calc R U . . .
C22 C 0.0417(7) 0.2900(6) 0.2962(4) 0.0162(15) Uani 1 1 d . . . . .
C23 C -0.0623(7) 0.2232(6) 0.3437(3) 0.0178(15) Uani 1 1 d . . . . .
C24 C 0.0067(7) 0.2085(6) 0.4145(3) 0.0161(14) Uani 1 1 d . . . . .
C25 C -0.0518(7) 0.1435(7) 0.4857(4) 0.0240(16) Uani 1 1 d . . . . .
H25A H -0.112474 0.051303 0.463348 0.036 Uiso 1 1 calc R U . . .
H25B H -0.105185 0.184103 0.515629 0.036 Uiso 1 1 calc R U . . .
H25C H 0.023687 0.151878 0.525190 0.036 Uiso 1 1 calc R U . . .
C26 C -0.2852(7) 0.0384(7) 0.2316(4) 0.0258(17) Uani 1 1 d . . . . .
C27 C -0.1952(8) -0.0101(7) 0.2000(4) 0.0303(18) Uani 1 1 d . . . . .
H27 H -0.101668 0.027455 0.224269 0.036 Uiso 1 1 calc R U . . .
C28 C -0.2452(9) -0.1150(8) 0.1320(4) 0.037(2) Uani 1 1 d . . . . .
H28 H -0.181570 -0.145173 0.109408 0.045 Uiso 1 1 calc R U . . .
C29 C -0.4597(9) -0.1287(9) 0.1269(5) 0.046(2) Uani 1 1 d . . . . .
H29 H -0.553423 -0.170407 0.102495 0.055 Uiso 1 1 calc R U . . .
C30 C -0.4198(8) -0.0203(8) 0.1934(4) 0.039(2) Uani 1 1 d . . . . .
H30 H -0.483958 0.011790 0.211679 0.046 Uiso 1 1 calc R U . . .
C31 C 0.8057(14) -0.0937(12) -0.1007(6) 0.086(4) Uani 1 1 d . . . . .
H31A H 0.826300 -0.084442 -0.038795 0.103 Uiso 1 1 calc R U . . .
H31B H 0.820851 -0.167429 -0.130340 0.103 Uiso 1 1 calc R U . . .
C32 C 0.6564(13) -0.1228(10) -0.1198(6) 0.079(3) Uani 1 1 d . . . . .
H32A H 0.596460 -0.202863 -0.101001 0.118 Uiso 1 1 calc R U . . .
H32B H 0.640544 -0.050774 -0.089644 0.118 Uiso 1 1 calc R U . . .
H32C H 0.635098 -0.133733 -0.181157 0.118 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
N8 Cu1 N1 169.2(2) . . ?
N8 Cu1 N3 96.64(19) . 2_656 ?
N1 Cu1 N3 94.07(18) . 2_656 ?
N2 Cu2 N4 170.9(2) . . ?
N5 Cu3 N7 175.6(2) . . ?
C3 S1 C6 102.7(3) . . ?
C13 S2 C16 103.5(3) . . ?
C23 S3 C26 103.4(3) . . ?
C2 N1 N2 109.1(5) . . ?
C2 N1 Cu1 131.2(5) . . ?
N2 N1 Cu1 116.5(3) . . ?
C4 N2 N1 107.7(5) . . ?
C4 N2 Cu2 129.7(4) . . ?
N1 N2 Cu2 122.3(4) . . ?
C9 N3 C8 116.9(5) . . ?
C9 N3 Cu1 117.6(4) . 2_656 ?
C8 N3 Cu1 122.7(4) . 2_656 ?
C12 N4 N5 108.3(5) . . ?
C12 N4 Cu2 133.7(4) . . ?
N5 N4 Cu2 118.0(4) . . ?
C14 N5 N4 107.9(5) . . ?
C14 N5 Cu3 133.3(4) . . ?
N4 N5 Cu3 118.6(4) . . ?
C18 N6 C19 115.7(6) . . ?
C22 N7 N8 108.6(5) . . ?
C22 N7 Cu3 128.8(4) . . ?
N8 N7 Cu3 122.4(4) . . ?
C24 N8 N7 108.7(5) . . ?
C24 N8 Cu1 135.8(4) . . ?
N7 N8 Cu1 115.3(4) . . ?
C29 N9 C28 115.8(7) . . ?
N1 C2 C3 107.5(6) . . ?
N1 C2 C1 121.7(6) . . ?
C3 C2 C1 130.8(5) . . ?
C4 C3 C2 106.7(5) . . ?
C4 C3 S1 125.6(5) . . ?
C2 C3 S1 127.6(5) . . ?
N2 C4 C3 109.0(6) . . ?
N2 C4 C5 121.2(5) . . ?
C3 C4 C5 129.8(5) . . ?
C10 C6 C7 117.6(6) . . ?
C10 C6 S1 123.4(5) . . ?
C7 C6 S1 119.0(5) . . ?
C6 C7 C8 118.9(6) . . ?
N3 C8 C7 123.1(6) . . ?
N3 C9 C10 123.6(6) . . ?
C9 C10 C6 119.8(6) . . ?
N4 C12 C13 108.5(5) . . ?
N4 C12 C11 121.8(5) . . ?
C13 C12 C11 129.7(6) . . ?
C14 C13 C12 106.4(5) . . ?
C14 C13 S2 125.7(4) . . ?
C12 C13 S2 127.9(5) . . ?
N5 C14 C13 108.9(5) . . ?
N5 C14 C15 120.9(6) . . ?
C13 C14 C15 130.2(6) . . ?
C17 C16 C20 117.3(6) . . ?
C17 C16 S2 125.8(5) . . ?
C20 C16 S2 116.8(6) . . ?
C18 C17 C16 119.6(7) . . ?
N6 C18 C17 124.4(8) . . ?
N6 C19 C20 124.5(7) . . ?
C19 C20 C16 118.4(8) . . ?
N7 C22 C23 109.1(5) . . ?
N7 C22 C21 121.1(6) . . ?
C23 C22 C21 129.7(6) . . ?
C22 C23 C24 105.4(5) . . ?
C22 C23 S3 126.5(5) . . ?
C24 C23 S3 128.2(5) . . ?
N8 C24 C23 108.2(5) . . ?
N8 C24 C25 122.4(5) . . ?
C23 C24 C25 129.5(6) . . ?
C30 C26 C27 118.0(7) . . ?
C30 C26 S3 117.8(6) . . ?
C27 C26 S3 124.2(5) . . ?
C28 C27 C26 118.4(7) . . ?
N9 C28 C27 124.8(8) . . ?
N9 C29 C30 124.4(7) . . ?
C26 C30 C29 118.5(8) . . ?
O1 C31 C32 112.0(8) . . ?
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 N8 1.902(5) . ?
Cu1 N1 1.909(5) . ?
Cu1 N3 2.308(5) 2_656 ?
Cu2 N2 1.847(5) . ?
Cu2 N4 1.855(5) . ?
Cu3 N5 1.848(5) . ?
Cu3 N7 1.853(5) . ?
S1 C3 1.751(6) . ?
S1 C6 1.770(6) . ?
S2 C13 1.744(6) . ?
S2 C16 1.758(7) . ?
S3 C23 1.741(6) . ?
S3 C26 1.784(7) . ?
O1 C31 1.474(13) . ?
N1 C2 1.344(7) . ?
N1 N2 1.394(7) . ?
N2 C4 1.343(7) . ?
N3 C9 1.332(7) . ?
N3 C8 1.337(8) . ?
N4 C12 1.336(8) . ?
N4 N5 1.391(7) . ?
N5 C14 1.347(7) . ?
N6 C18 1.336(9) . ?
N6 C19 1.346(10) . ?
N7 C22 1.338(7) . ?
N7 N8 1.376(6) . ?
N8 C24 1.337(8) . ?
N9 C29 1.321(10) . ?
N9 C28 1.332(9) . ?
C1 C2 1.468(9) . ?
C2 C3 1.405(8) . ?
C3 C4 1.387(8) . ?
C4 C5 1.490(9) . ?
C6 C10 1.377(8) . ?
C6 C7 1.386(8) . ?
C7 C8 1.393(9) . ?
C9 C10 1.371(8) . ?
C11 C12 1.493(9) . ?
C12 C13 1.400(8) . ?
C13 C14 1.379(9) . ?
C14 C15 1.495(8) . ?
C16 C17 1.382(10) . ?
C16 C20 1.406(9) . ?
C17 C18 1.372(9) . ?
C19 C20 1.376(10) . ?
C21 C22 1.511(8) . ?
C22 C23 1.388(9) . ?
C23 C24 1.418(8) . ?
C24 C25 1.479(9) . ?
C26 C30 1.380(9) . ?
C26 C27 1.386(9) . ?
C27 C28 1.388(9) . ?
C29 C30 1.404(10) . ?
C31 C32 1.506(15) . ?
