#------------------------------------------------------------------------------
#$Date: 2025-08-23 00:35:05 +0200 (Sat 23 de Aug de 2025) $
#$Revision: 301870 $
#$URL: svn://www.crystallography.net/cod/cif/7/24/25/7242551.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_7242551
loop_
_publ_author_name
'Klongdee, Fatima'
'Leelasubcharoen, Somying'
'Youngme, Sujittra'
'Boonmak, Jaursup'
_publ_section_title
;
 Sonochemical synthesis of a trinuclear Cu(ii) complex with open
 coordination sites for the differentiable optical detection of volatile
 amines
;
_journal_issue                   20
_journal_name_full               'RSC Advances'
_journal_page_first              12218
_journal_page_last               12226
_journal_paper_doi               10.1039/D1RA01151K
_journal_volume                  11
_journal_year                    2021
_chemical_formula_moiety         'C30 H28 Cu3 N10 O12'
_chemical_formula_sum            'C30 H28 Cu3 N10 O12'
_chemical_formula_weight         911.24
_chemical_name_common
{tetraaqua-bis(2,2'-dipyridylamine)-bis(mu-pyrazole-3,5-dicarbarboxylato)tricopper(II)}
_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   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2021-02-09 deposited with the CCDC.	2021-03-11 downloaded from the CCDC.
;
_cell_angle_alpha                106.045(6)
_cell_angle_beta                 104.318(7)
_cell_angle_gamma                99.588(6)
_cell_formula_units_Z            1
_cell_length_a                   7.5789(18)
_cell_length_b                   9.937(2)
_cell_length_c                   11.529(3)
_cell_measurement_reflns_used    1789
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      23.228
_cell_measurement_theta_min      3.381
_cell_volume                     782.4(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       BrukerAPEX2
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    SHELXL
_computing_publication_material  SHELXL
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type
;
Bruker D8 QUEST PHOTON 100
;
_diffrn_measurement_method       '\fandω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1232
_diffrn_reflns_av_unetI/netI     0.1164
_diffrn_reflns_Laue_measured_fraction_full 0.901
_diffrn_reflns_Laue_measured_fraction_max 0.901
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9594
_diffrn_reflns_point_group_measured_fraction_full 0.901
_diffrn_reflns_point_group_measured_fraction_max 0.901
_diffrn_reflns_theta_full        24.511
_diffrn_reflns_theta_max         24.511
_diffrn_reflns_theta_min         3.145
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.107
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.6142
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2012/1
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.934
_exptl_crystal_description       block
_exptl_crystal_F_000             461
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.072
_refine_diff_density_min         -1.168
_refine_diff_density_rms         0.198
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         2359
_refine_ls_number_restraints     214
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1535
_refine_ls_R_factor_gt           0.0894
_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)+(0.1442P)²+4.1594P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2246
_refine_ls_wR_factor_ref         0.2598
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1465
_reflns_number_total             2359
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1ra01151k2.cif
_cod_data_source_block           Cupzdcdpyam1_a
_cod_database_code               7242551
_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   0.866
_shelx_estimated_absorpt_t_max   0.939
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 0.5000 0.5000 0.5000 0.0308(7) Uani 1 2 d S . P . .
Cu2 Cu 0.5176(3) 0.23749(18) 0.75221(16) 0.0359(6) Uani 1 1 d D . . . .
O1 O 0.6403(13) 0.0603(9) 0.7207(8) 0.031(2) Uani 1 1 d . U . . .
O2 O 0.8089(13) -0.0432(9) 0.6046(8) 0.035(2) Uani 1 1 d . U . . .
O3 O 0.6568(12) 0.4925(8) 0.3843(8) 0.0258(19) Uani 1 1 d . U . . .
O4 O 0.8630(12) 0.3785(9) 0.3196(8) 0.028(2) Uani 1 1 d . U . . .
O5 O 0.2523(13) 0.2311(10) 0.6394(9) 0.031(2) Uani 1 1 d D . . . .
O6 O 0.2255(13) 0.3011(9) 0.3405(9) 0.036(2) Uani 1 1 d D . . . .
H6 H 0.282(14) 0.301(7) 0.614(9) 0.05(5) Uiso 1 1 d D . . . .
N1 N 0.4095(15) 0.1721(10) 0.8767(10) 0.025(2) Uani 1 1 d . U . . .
N2 N 0.6600(15) 0.4270(10) 0.8963(10) 0.027(2) Uani 1 1 d . U . . .
N3 N 0.6512(15) 0.3244(11) 1.0581(10) 0.028(2) Uani 1 1 d . U . . .
H3 H 0.7181 0.3249 1.1304 0.034 Uiso 1 1 calc R U . . .
N4 N 0.6196(14) 0.2605(9) 0.6129(9) 0.0200(19) Uani 1 1 d . U . . .
N5 N 0.6282(14) 0.3528(10) 0.5459(9) 0.022(2) Uani 1 1 d . U . . .
C1 C 0.4961(18) 0.2141(13) 1.0015(12) 0.024(2) Uani 1 1 d . U . . .
C2 C 0.4296(19) 0.1409(13) 1.0755(13) 0.028(2) Uani 1 1 d . U . . .
H2 H 0.4940 0.1675 1.1616 0.034 Uiso 1 1 calc R U . . .
C3 C 0.2724(19) 0.0317(13) 1.0226(12) 0.028(2) Uani 1 1 d . U . . .
H3A H 0.2273 -0.0172 1.0716 0.034 Uiso 1 1 calc R U . . .
C4 C 0.1779(19) -0.0074(14) 0.8931(13) 0.031(2) Uani 1 1 d . U . . .
H4 H 0.0681 -0.0816 0.8548 0.037 Uiso 1 1 calc R U . . .
C5 C 0.2490(19) 0.0648(12) 0.8247(13) 0.028(2) Uani 1 1 d . U . . .
H5 H 0.1853 0.0398 0.7387 0.034 Uiso 1 1 calc R U . . .
C6 C 0.7239(17) 0.4397(12) 1.0199(12) 0.022(2) Uani 1 1 d . U . . .
C7 C 0.8576(18) 0.5575(13) 1.1081(12) 0.027(2) Uani 1 1 d . U . . .
H7 H 0.8973 0.5630 1.1927 0.033 Uiso 1 1 calc R U . . .
C8 C 0.9311(19) 0.6654(14) 1.0713(12) 0.029(2) Uani 1 1 d . U . . .
H8 H 1.0265 0.7439 1.1295 0.035 Uiso 1 1 calc R U . . .
C9 C 0.8646(18) 0.6588(13) 0.9471(12) 0.029(2) Uani 1 1 d . U . . .
H9 H 0.9105 0.7349 0.9216 0.034 Uiso 1 1 calc R U . . .
C10 C 0.7315(18) 0.5406(13) 0.8620(13) 0.029(2) Uani 1 1 d . U . . .
H10 H 0.6875 0.5367 0.7780 0.035 Uiso 1 1 calc R U . . .
C11 C 0.7268(17) 0.1682(12) 0.5796(11) 0.021(2) Uani 1 1 d . U . . .
C12 C 0.8017(17) 0.1994(12) 0.4925(11) 0.023(2) Uani 1 1 d . U . . .
H12 H 0.8794 0.1526 0.4541 0.027 Uiso 1 1 calc R U . . .
C13 C 0.7370(17) 0.3166(12) 0.4729(11) 0.022(2) Uani 1 1 d . U . . .
C14 C 0.7277(18) 0.0523(12) 0.6393(12) 0.025(2) Uani 1 1 d . U . . .
C15 C 0.7600(18) 0.4004(13) 0.3862(11) 0.025(2) Uani 1 1 d . U . . .
H1 H 0.239(16) 0.158(7) 0.576(6) 0.05(5) Uiso 1 1 d D . . . .
H11 H 0.134(3) 0.349(3) 0.336(9) 0.04(4) Uiso 1 1 d D . . . .
H13 H 0.183(6) 0.207(2) 0.330(8) 0.25(17) Uiso 1 1 d D . . . .
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'
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
O3 Cu1 O3 180.0 . 2_666 ?
O3 Cu1 N5 97.2(3) . 2_666 ?
O3 Cu1 N5 82.8(3) 2_666 2_666 ?
O3 Cu1 N5 82.8(3) . . ?
O3 Cu1 N5 97.2(3) 2_666 . ?
N5 Cu1 N5 180.0 2_666 . ?
N4 Cu2 N1 168.6(4) . . ?
N4 Cu2 N2 101.9(4) . . ?
N1 Cu2 N2 87.8(4) . . ?
N4 Cu2 O5 88.5(4) . . ?
N1 Cu2 O5 92.2(4) . . ?
N2 Cu2 O5 116.9(4) . . ?
N4 Cu2 O1 79.5(3) . . ?
N1 Cu2 O1 90.7(3) . . ?
N2 Cu2 O1 120.3(4) . . ?
O5 Cu2 O1 122.8(4) . . ?
C14 O1 Cu2 114.5(6) . . ?
C15 O3 Cu1 114.5(6) . . ?
Cu2 O5 H6 99(7) . . ?
Cu2 O5 H1 99(7) . . ?
H6 O5 H1 103(5) . . ?
H11 O6 H13 112.89(19) . . ?
C1 N1 C5 119.2(10) . . ?
C1 N1 Cu2 124.7(9) . . ?
C5 N1 Cu2 115.6(8) . . ?
C6 N2 C10 116.9(12) . . ?
C6 N2 Cu2 124.8(8) . . ?
C10 N2 Cu2 116.6(8) . . ?
C1 N3 C6 131.4(11) . . ?
C1 N3 H3 114.3 . . ?
C6 N3 H3 114.3 . . ?
N5 N4 C11 107.1(8) . . ?
N5 N4 Cu2 137.9(7) . . ?
C11 N4 Cu2 114.6(7) . . ?
C13 N5 N4 108.0(8) . . ?
C13 N5 Cu1 110.7(7) . . ?
N4 N5 Cu1 140.3(7) . . ?
N1 C1 N3 121.3(10) . . ?
N1 C1 C2 120.3(12) . . ?
N3 C1 C2 118.4(12) . . ?
C3 C2 C1 120.1(12) . . ?
C3 C2 H2 120.0 . . ?
C1 C2 H2 120.0 . . ?
C2 C3 C4 119.2(11) . . ?
C2 C3 H3A 120.4 . . ?
C4 C3 H3A 120.4 . . ?
C5 C4 C3 118.7(13) . . ?
C5 C4 H4 120.7 . . ?
C3 C4 H4 120.7 . . ?
C4 C5 N1 122.4(13) . . ?
C4 C5 H5 118.8 . . ?
N1 C5 H5 118.8 . . ?
N2 C6 C7 122.7(11) . . ?
N2 C6 N3 118.1(12) . . ?
C7 C6 N3 119.2(11) . . ?
C8 C7 C6 119.3(12) . . ?
C8 C7 H7 120.3 . . ?
C6 C7 H7 120.3 . . ?
C7 C8 C9 119.6(14) . . ?
C7 C8 H8 120.2 . . ?
C9 C8 H8 120.2 . . ?
C10 C9 C8 119.5(12) . . ?
C10 C9 H9 120.2 . . ?
C8 C9 H9 120.2 . . ?
C9 C10 N2 121.8(12) . . ?
C9 C10 H10 119.1 . . ?
N2 C10 H10 119.1 . . ?
C12 C11 N4 110.4(9) . . ?
C12 C11 C14 134.2(10) . . ?
N4 C11 C14 115.3(9) . . ?
C11 C12 C13 104.8(9) . . ?
C11 C12 H12 127.6 . . ?
C13 C12 H12 127.6 . . ?
N5 C13 C12 109.8(9) . . ?
N5 C13 C15 117.3(9) . . ?
C12 C13 C15 132.9(10) . . ?
O2 C14 O1 125.8(10) . . ?
O2 C14 C11 118.6(10) . . ?
O1 C14 C11 115.5(9) . . ?
O4 C15 O3 123.9(10) . . ?
O4 C15 C13 121.7(10) . . ?
O3 C15 C13 114.3(9) . . ?
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 O3 1.989(7) . ?
Cu1 O3 1.989(7) 2_666 ?
Cu1 N5 2.003(9) 2_666 ?
Cu1 N5 2.003(9) . ?
Cu2 N4 1.997(9) . ?
Cu2 N1 2.018(9) . ?
Cu2 N2 2.044(11) . ?
Cu2 O5 2.088(10) . ?
Cu2 O1 2.111(8) . ?
O1 C14 1.269(14) . ?
O2 C14 1.244(13) . ?
O3 C15 1.300(13) . ?
O4 C15 1.228(13) . ?
O5 H6 0.84(2) . ?
O5 H1 0.85(2) . ?
O6 H11 0.9000(11) . ?
O6 H13 0.9000(11) . ?
N1 C1 1.336(16) . ?
N1 C5 1.353(16) . ?
N2 C6 1.349(15) . ?
N2 C10 1.369(15) . ?
N3 C1 1.343(16) . ?
N3 C6 1.414(14) . ?
N3 H3 0.8600 . ?
N4 N5 1.355(12) . ?
N4 C11 1.362(14) . ?
N5 C13 1.339(14) . ?
C1 C2 1.396(16) . ?
C2 C3 1.347(18) . ?
C2 H2 0.9300 . ?
C3 C4 1.396(18) . ?
C3 H3A 0.9300 . ?
C4 C5 1.349(16) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C6 C7 1.367(18) . ?
C7 C8 1.345(17) . ?
C7 H7 0.9300 . ?
C8 C9 1.374(18) . ?
C8 H8 0.9300 . ?
C9 C10 1.356(18) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 C12 1.350(15) . ?
C11 C14 1.495(15) . ?
C12 C13 1.389(15) . ?
C12 H12 0.9300 . ?
C13 C15 1.490(15) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 168342089
