#------------------------------------------------------------------------------
#$Date: 2025-08-21 16:09:30 +0200 (Thu 21 de Aug de 2025) $
#$Revision: 301850 $
#$URL: svn://www.crystallography.net/cod/cif/7/04/29/7042948.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_7042948
loop_
_publ_author_name
'Gong, Yun-Nan'
'Wei, Xue-Wen'
'He, Lv-Heng'
'Wen, Ya-Qiong'
'Ren, Ya-Wen'
'Xie, Yong-Rong'
'Zhong, Di-Chang'
_publ_section_title
;
 Two bilayer metal−organic frameworks with rare trinuclear
 heterometal clusters and tunable photoluminescence
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01242J
_journal_year                    2017
_chemical_formula_moiety         'C42 H18 Cl2 K O12 Pb2, 3(C2 H8 N)'
_chemical_formula_sum            'C48 H42 Cl2 K N3 O12 Pb2'
_chemical_formula_weight         1377.22
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-04-25
_audit_creation_method
;
Olex2 1.2-dev
(compiled 2017.03.14 svn.r3397 for OlexSys, GUI svn.r3563)
;
_audit_update_record
;
2017-05-04 deposited with the CCDC.
2017-05-12 downloaded from the CCDC.
;
_cell_angle_alpha                107.383(2)
_cell_angle_beta                 108.957(2)
_cell_angle_gamma                91.213(3)
_cell_formula_units_Z            1
_cell_length_a                   9.9175(5)
_cell_length_b                   10.0625(4)
_cell_length_c                   13.4072(7)
_cell_measurement_reflns_used    4414
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.34
_cell_measurement_theta_min      2.85
_cell_volume                     1197.20(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10094
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.503
_diffrn_reflns_theta_min         2.190
_exptl_absorpt_coefficient_mu    7.286
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4628
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.1113 before and 0.0311 after correction. The Ratio of minimum to maximum transmission is 0.6207. The λ/2 correction factor is 0.0015.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.910
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.170
_refine_diff_density_min         -1.112
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         5386
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0371
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0311P)²+3.4908P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0794
_refine_ls_wR_factor_ref         0.0831
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4666
_reflns_number_total             5386
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7dt01242j2.cif
_cod_data_source_block           1
_cod_database_code               7042948
_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.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N24-C3 \\sim N24-C1A
 with sigma of 0.0001
 C22-C23 \\sim C3-C1A
 with sigma of 0.001
3. Rigid body (RIGU) restrains
 N24, C3, C1A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: C3(0.5) H3A(0.5) H3B(0.5) H3C(0.5) N24(0.5) H24A(0.5) H24B(0.5)
 C1A(0.5) H1AA(0.5) H1AB(0.5) H1AC(0.5)
5.a Secondary CH2 refined with riding coordinates:
 N24(H24A,H24B), N2(H2A,H2B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C7(H7), C8(H8), C9(H9), C11(H11), C15(H15), C16(H16), C18(H18)
5.c Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C3(H3A,H3B,H3C), C1A(H1AA,H1AB,H1AC)
;
_olex2_submission_special_instructions 'No special instructions were received'
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
C1 C 0.5729(5) -0.0320(5) 0.3400(4) 0.0305(11) Uani 1 1 d . . . . .
C2 C 0.8916(6) -0.0007(6) 0.6006(5) 0.0405(13) Uani 1 1 d . . . . .
H2 H 0.9386 -0.0747 0.5738 0.049 Uiso 1 1 calc R . . . .
C0AA C 0.7022(5) -0.0605(6) 0.4096(4) 0.0319(11) Uani 1 1 d . . . . .
C4 C 0.7627(6) -0.1791(6) 0.3648(4) 0.0360(12) Uani 1 1 d . . . . .
H4 H 0.8480 -0.1989 0.4097 0.043 Uiso 1 1 calc R . . . .
C5 C 0.5093(5) 0.0942(5) 0.3826(4) 0.0303(11) Uani 1 1 d . . . . .
C6 C 0.7026(6) 0.1457(5) 0.5683(4) 0.0326(11) Uani 1 1 d . . . . .
C7 C 0.5080(6) -0.1258(6) 0.2320(5) 0.0384(13) Uani 1 1 d . . . . .
H7 H 0.4209 -0.1096 0.1868 0.046 Uiso 1 1 calc R . . . .
C8 C 0.7596(6) 0.2234(6) 0.6818(4) 0.0381(13) Uani 1 1 d . . . . .
H8 H 0.7168 0.3006 0.7093 0.046 Uiso 1 1 calc R . . . .
C9 C 0.3859(6) 0.1306(6) 0.3134(4) 0.0354(12) Uani 1 1 d . . . . .
H9 H 0.3435 0.0737 0.2395 0.042 Uiso 1 1 calc R . . . .
C10 C 0.5745(6) 0.1809(5) 0.4938(5) 0.0343(12) Uani 1 1 d . . . . .
C11 C 0.9436(6) 0.0769(7) 0.7114(5) 0.0436(14) Uani 1 1 d . . . . .
H11 H 1.0247 0.0541 0.7587 0.052 Uiso 1 1 calc R . . . .
C12 C 0.1976(6) 0.2882(7) 0.2757(5) 0.0423(14) Uani 1 1 d . . . . .
C13 C 0.3265(6) 0.2498(6) 0.3533(4) 0.0351(12) Uani 1 1 d . . . . .
C14 C 0.7682(6) 0.0294(6) 0.5262(5) 0.0339(12) Uani 1 1 d . . . . .
C15 C 0.5690(6) -0.2411(6) 0.1907(5) 0.0380(13) Uani 1 1 d . . . . .
H15 H 0.5230 -0.3019 0.1186 0.046 Uiso 1 1 calc R . . . .
C16 C 0.3909(7) 0.3342(6) 0.4632(5) 0.0461(15) Uani 1 1 d . . . . .
H16 H 0.3519 0.4144 0.4907 0.055 Uiso 1 1 calc R . . . .
C17 C 0.8768(6) 0.1893(6) 0.7542(5) 0.0383(13) Uani 1 1 d . . . . .
C18 C 0.5104(7) 0.3011(6) 0.5315(5) 0.0450(15) Uani 1 1 d . . . . .
H18 H 0.5512 0.3591 0.6051 0.054 Uiso 1 1 calc R . . . .
C19 C 0.6998(6) -0.2671(6) 0.2565(5) 0.0368(12) Uani 1 1 d . . . . .
C20 C 0.9250(7) 0.2701(7) 0.8763(5) 0.0464(15) Uani 1 1 d . . . . .
C21 C 0.7733(7) -0.3876(6) 0.2111(5) 0.0430(14) Uani 1 1 d . . . . .
C22 C 0.6163(11) 0.8319(8) 0.9727(8) 0.087(3) Uani 1 1 d D . . . .
H22A H 0.6079 0.8705 0.9139 0.130 Uiso 1 1 calc GR . . . .
H22B H 0.6815 0.8951 1.0417 0.130 Uiso 1 1 calc GR . . . .
H22C H 0.5236 0.8188 0.9789 0.130 Uiso 1 1 calc GR . . . .
C23 C 0.5755(12) 0.5860(9) 0.8500(8) 0.106(4) Uani 1 1 d D . . . .
H23A H 0.4875 0.5668 0.8615 0.158 Uiso 1 1 calc GR . . . .
H23B H 0.6215 0.5025 0.8388 0.158 Uiso 1 1 calc GR . . . .
H23C H 0.5550 0.6158 0.7855 0.158 Uiso 1 1 calc GR . . . .
C3 C 0.0670(19) 0.6165(3) 0.536(2) 0.072(5) Uani 0.5 1 d D U . A -1
H3A H 0.0285 0.6418 0.4699 0.108 Uiso 0.5 1 calc GR . . A -1
H3B H 0.1676 0.6516 0.5713 0.108 Uiso 0.5 1 calc GR . . A -1
H3C H 0.0174 0.6564 0.5866 0.108 Uiso 0.5 1 calc GR . . A -1
Cl1 Cl -0.2264(3) 0.1858(3) 0.0808(3) 0.1102(10) Uani 1 1 d . . . . .
K1 K 0.0000 0.0000 0.0000 0.0455(4) Uani 1 2 d S T P . .
N24 N 0.0478(4) 0.4612(3) 0.5067(9) 0.068(3) Uani 0.5 1 d D U . A -1
H24A H 0.0916 0.4379 0.5673 0.082 Uiso 0.5 1 calc R . . A -1
H24B H 0.0893 0.4243 0.4568 0.082 Uiso 0.5 1 calc R . . A -1
N2 N 0.6709(6) 0.6970(6) 0.9476(5) 0.0544(14) Uani 1 1 d . . . . .
H2A H 0.6890 0.6679 1.0066 0.065 Uiso 1 1 calc R . . . .
H2B H 0.7540 0.7099 0.9376 0.065 Uiso 1 1 calc R . . . .
O1 O 0.1334(6) 0.3824(6) 0.3178(4) 0.0745(17) Uani 1 1 d . . . . .
O2 O 0.1614(4) 0.2268(5) 0.1732(3) 0.0506(11) Uani 1 1 d . . . . .
O3 O 0.8664(6) 0.3770(5) 0.9066(4) 0.0729(16) Uani 1 1 d . . . . .
O4 O 1.0205(5) 0.2275(5) 0.9418(4) 0.0555(12) Uani 1 1 d . . . . .
O5 O 0.8657(5) -0.4337(5) 0.2770(4) 0.0586(13) Uani 1 1 d . . . . .
O6 O 0.7390(5) -0.4387(5) 0.1073(4) 0.0565(12) Uani 1 1 d . . . . .
Pb1 Pb -0.04345(2) 0.40500(2) 0.12366(2) 0.03837(8) Uani 1 1 d . . . . .
C1A C -0.1061(4) 0.4007(10) 0.460(3) 0.080(6) Uani 0.5 1 d D U . A -1
H1AA H -0.1510 0.4150 0.3899 0.119 Uiso 0.5 1 calc GR . . A -1
H1AB H -0.1534 0.4461 0.5111 0.119 Uiso 0.5 1 calc GR . . A -1
H1AC H -0.1133 0.3019 0.4502 0.119 Uiso 0.5 1 calc GR . . 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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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'
Pb Pb -3.3944 10.1111 '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
C0AA C1 C5 119.7(5) . .
C7 C1 C0AA 118.6(5) . .
C7 C1 C5 121.7(5) . .
C11 C2 C14 121.3(5) . .
C1 C0AA C14 120.4(4) . .
C4 C0AA C1 118.1(5) . .
C4 C0AA C14 121.5(5) . .
C19 C4 C0AA 122.2(5) . .
C9 C5 C1 121.1(5) . .
C10 C5 C1 119.4(4) . .
C10 C5 C9 119.4(4) . .
C8 C6 C10 121.2(5) . .
C8 C6 C14 119.0(5) . .
C14 C6 C10 119.7(5) . .
C15 C7 C1 121.9(5) . .
C17 C8 C6 122.3(5) . .
C13 C9 C5 121.2(5) . .
C5 C10 C6 120.9(4) . .
C5 C10 C18 117.7(5) . .
C18 C10 C6 121.3(5) . .
C2 C11 C17 121.0(5) . .
O1 C12 C13 117.6(5) . .
O2 C12 C13 119.0(5) . .
O2 C12 O1 123.4(5) . .
C9 C13 C12 119.6(5) . .
C16 C13 C9 119.0(5) . .
C16 C13 C12 121.3(5) . .
C2 C14 C0AA 122.2(5) . .
C2 C14 C6 118.0(5) . .
C6 C14 C0AA 119.6(5) . .
C7 C15 C19 120.1(5) . .
C18 C16 C13 120.8(5) . .
C8 C17 C11 118.3(5) . .
C8 C17 C20 119.4(5) . .
C11 C17 C20 122.3(5) . .
C16 C18 C10 121.9(5) . .
C4 C19 C15 118.9(5) . .
C4 C19 C21 119.9(5) . .
C15 C19 C21 121.2(5) . .
O3 C20 C17 118.0(5) . .
O4 C20 C17 118.3(6) . .
O4 C20 O3 123.8(6) . .
O5 C21 C19 119.6(5) . .
O5 C21 O6 122.3(5) . .
O6 C21 C19 118.0(5) . .
Pb1 Cl1 K1 86.27(6) . .
Cl1 K1 Cl1 180.0 . 2
Cl1 K1 Pb1 139.19(4) 2 .
Cl1 K1 Pb1 139.19(4) . 2
Cl1 K1 Pb1 40.81(4) 2 2
Cl1 K1 Pb1 40.81(4) . .
O2 K1 Cl1 74.53(10) . .
O2 K1 Cl1 105.47(10) 2 .
O2 K1 Cl1 105.47(10) . 2
O2 K1 Cl1 74.53(10) 2 2
O2 K1 O2 180.0 2 .
O2 K1 Pb1 44.03(8) . .
O2 K1 Pb1 135.97(8) . 2
O2 K1 Pb1 135.97(8) 2 .
O2 K1 Pb1 44.03(8) 2 2
O4 K1 Cl1 104.54(12) 2_656 .
O4 K1 Cl1 75.46(12) 1_454 .
O4 K1 Cl1 104.55(12) 1_454 2
O4 K1 Cl1 75.45(12) 2_656 2
O4 K1 O2 66.85(13) 2_656 2
O4 K1 O2 66.85(13) 1_454 .
O4 K1 O2 113.15(13) 1_454 2
O4 K1 O2 113.15(13) 2_656 .
O4 K1 O4 180.0 2_656 1_454
O4 K1 Pb1 135.25(10) 1_454 2
O4 K1 Pb1 44.75(10) 2_656 2
O4 K1 Pb1 135.25(10) 2_656 .
O4 K1 Pb1 44.75(10) 1_454 .
Pb1 K1 Pb1 180.0 2 .
C3 N24 C1A 112.4(7) . .
C22 N2 C23 115.4(7) . .
C12 O1 Pb1 96.5(4) . .
C12 O2 K1 144.9(4) . .
C20 O3 Pb1 97.1(4) . 1_656
C20 O4 K1 128.0(4) . 1_656
C21 O5 Pb1 95.2(4) . 1_645
C21 O6 Pb1 92.7(3) . 1_645
Cl1 Pb1 O1 94.58(16) . .
Cl1 Pb1 O3 89.86(16) . 1_454
Cl1 Pb1 O5 93.57(13) . 1_465
Cl1 Pb1 O6 88.98(13) . 1_465
O3 Pb1 O1 156.61(15) 1_454 .
O3 Pb1 O6 78.88(14) 1_454 1_465
O5 Pb1 O1 75.31(13) 1_465 .
O5 Pb1 O3 127.38(14) 1_465 1_454
O5 Pb1 O6 48.77(13) 1_465 1_465
O6 Pb1 O1 124.08(13) 1_465 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C0AA 1.413(7) .
C1 C5 1.473(6) .
C1 C7 1.398(7) .
C2 C11 1.369(8) .
C2 C14 1.409(7) .
C0AA C4 1.408(7) .
C0AA C14 1.469(7) .
C4 C19 1.378(8) .
C5 C9 1.406(7) .
C5 C10 1.405(7) .
C6 C8 1.399(7) .
C6 C10 1.464(7) .
C6 C14 1.410(7) .
C7 C15 1.372(7) .
C8 C17 1.376(8) .
C9 C13 1.388(7) .
C10 C18 1.414(7) .
C11 C17 1.393(8) .
C12 C13 1.504(7) .
C12 O1 1.250(7) .
C12 O2 1.249(7) .
C13 C16 1.386(8) .
C15 C19 1.392(8) .
C16 C18 1.359(8) .
C17 C20 1.499(8) .
C19 C21 1.502(7) .
C20 O3 1.256(8) .
C20 O4 1.246(7) .
C21 O5 1.254(7) .
C21 O6 1.256(7) .
C22 N2 1.457(9) .
C23 N2 1.460(9) .
C3 N24 1.484(4) .
Cl1 K1 3.202(2) .
Cl1 Pb1 2.623(2) .
K1 Cl1 3.202(2) 2
K1 O2 2.725(4) 2
K1 O2 2.725(4) .
K1 O4 2.654(5) 1_454
K1 O4 2.654(5) 2_656
K1 Pb1 4.0055(3) 2
K1 Pb1 4.0055(3) .
N24 C1A 1.484(4) .
O1 Pb1 2.704(5) .
O3 Pb1 2.675(5) 1_656
O4 K1 2.654(5) 1_656
O5 Pb1 2.636(4) 1_645
O6 Pb1 2.687(4) 1_645
Pb1 O3 2.675(5) 1_454
Pb1 O5 2.636(4) 1_465
Pb1 O6 2.687(4) 1_465
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139170741
