# Supplementary Information (SI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2025

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 2375275'
loop_
_audit_author_name
_audit_author_address
'Patrizia Rossi'
;University of Firenze
Italy
;
_audit_update_record             
;
2024-10-17 deposited with the CCDC.	2024-12-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H28 Cl2 Cu N5 O8.50'
_chemical_formula_weight         584.89

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y+1/2, z'
'-y+3/4, x+1/4, z+1/4'
'y+1/4, -x+1/4, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'y+3/4, -x+3/4, z+3/4'
'-x, -y, -z'
'x, y-1/2, -z'
'y-3/4, -x-1/4, -z-1/4'
'-y-1/4, x-1/4, -z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'-y+1/4, x+1/4, -z+1/4'

_cell_length_a                   17.3117(3)
_cell_length_b                   17.3117(3)
_cell_length_c                   31.2201(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     9356.5(4)
_cell_formula_units_Z            16
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2376
_cell_measurement_theta_min      4.5
_cell_measurement_theta_max      65

_exptl_crystal_description       prismatic
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.661
_exptl_crystal_F_000             4832
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    3.939
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.38
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.5418
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Onyx'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            10064
_diffrn_reflns_av_unetI/netI     0.0468
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         4.590
_diffrn_reflns_theta_max         71.151
_diffrn_reflns_theta_full        67.680
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             4416
_reflns_number_gt                2874
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_cell_refinement       
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_data_reduction        
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_structure_solution    'SIR97 (Altomare 1997)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Mercury 3.10.1'
_computing_publication_material  'PARST(Nardelli, 1995)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0848P)²+12.9565P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4416
_refine_ls_number_parameters     384
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0944
_refine_ls_R_factor_gt           0.0579
_refine_ls_wR_factor_ref         0.1766
_refine_ls_wR_factor_gt          0.1477
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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 0.73800(4) 0.12289(4) 0.54425(2) 0.0538(2) Uani 1 1 d . . . . .
Cl1 Cl 0.51798(8) -0.05095(10) 0.59540(4) 0.0745(4) Uani 1 1 d . . . . .
Cl2 Cl 0.88314(9) 0.39834(8) 0.54484(4) 0.0705(4) Uani 1 1 d . . . . .
N3 N 0.7161(2) 0.1477(3) 0.48077(11) 0.0584(10) Uani 1 1 d . . . . .
N2 N 0.8355(2) 0.1850(3) 0.53680(12) 0.0599(10) Uani 1 1 d . . . . .
H2 H 0.825132 0.239961 0.541825 0.072 Uiso 1 1 calc R U . . .
N5 N 0.6526(2) 0.2109(2) 0.55293(11) 0.0505(9) Uani 1 1 d . . . . .
C4 C 0.6328(3) 0.2474(3) 0.59090(14) 0.0503(11) Uani 1 1 d . . . . .
C31 C 0.6257(3) 0.2381(3) 0.51650(15) 0.0564(12) Uani 1 1 d . . . . .
N4 N 0.6831(3) 0.0223(3) 0.53445(14) 0.0744(13) Uani 1 1 d . . . . .
H4 H 0.636118 0.021644 0.551942 0.089 Uiso 1 1 calc R U . . .
C30 C 0.5564(3) 0.3399(3) 0.5516(2) 0.0714(15) Uani 1 1 d . . . . .
H30 H 0.524106 0.382813 0.550547 0.086 Uiso 1 1 calc R U . . .
C6 C 0.5779(3) 0.3036(3) 0.51476(18) 0.0647(14) Uani 1 1 d . . . . .
H6A H 0.560879 0.322226 0.488447 0.078 Uiso 1 1 calc R U . . .
C7 C 0.6628(3) 0.2196(3) 0.62954(14) 0.0592(12) Uani 1 1 d . . . . .
H7 H 0.695489 0.176944 0.629467 0.071 Uiso 1 1 calc R U . . .
C29 C 0.5836(3) 0.3118(3) 0.59132(17) 0.0569(12) Uani 1 1 d . . . . .
N1 N 0.7971(3) 0.0666(3) 0.59073(14) 0.0726(13) Uani 1 1 d . . . . .
H1 H 0.790365 0.093168 0.618207 0.087 Uiso 1 1 calc R U . . .
C10 C 0.5648(3) 0.3453(3) 0.6316(2) 0.0742(16) Uani 1 1 d . . . . .
H10 H 0.531033 0.387096 0.632595 0.089 Uiso 1 1 calc R U . . .
C11 C 0.6439(3) 0.1920(4) 0.47635(15) 0.0684(15) Uani 1 1 d . . . . .
H11A H 0.601650 0.156718 0.470499 0.082 Uiso 1 1 calc R U . . .
H11B H 0.648415 0.226985 0.452219 0.082 Uiso 1 1 calc R U . . .
C12 C 0.7831(3) 0.1923(3) 0.46537(15) 0.0651(14) Uani 1 1 d . . . . .
H12A H 0.772664 0.247172 0.468098 0.078 Uiso 1 1 calc R U . . .
H12B H 0.792252 0.181066 0.435358 0.078 Uiso 1 1 calc R U . . .
C13 C 0.6442(3) 0.2547(3) 0.66750(15) 0.0666(14) Uani 1 1 d . . . . .
H13 H 0.664898 0.235954 0.692934 0.080 Uiso 1 1 calc R U . . .
C14 C 0.8537(3) 0.1716(3) 0.49123(16) 0.0649(13) Uani 1 1 d . . . . .
H14A H 0.867205 0.117849 0.486660 0.078 Uiso 1 1 calc R U . . .
H14B H 0.897177 0.203378 0.482594 0.078 Uiso 1 1 calc R U . . .
C15 C 0.5950(3) 0.3177(4) 0.66852(19) 0.0751(16) Uani 1 1 d . . . . .
H15 H 0.582680 0.340909 0.694503 0.090 Uiso 1 1 calc R U . . .
C16 C 0.7108(4) 0.0694(4) 0.46101(17) 0.0792(17) Uani 1 1 d . . . . .
H16A H 0.762208 0.047671 0.458039 0.095 Uiso 1 1 calc R U . . .
H16B H 0.688192 0.073464 0.432681 0.095 Uiso 1 1 calc R U . . .
C17 C 0.6610(4) 0.0160(4) 0.4891(2) 0.091(2) Uani 1 1 d . . . . .
H17A H 0.606978 0.029891 0.485858 0.110 Uiso 1 1 calc R U . . .
H17B H 0.667196 -0.036989 0.479669 0.110 Uiso 1 1 calc R U . . .
C18 C 0.8946(3) 0.1567(4) 0.5671(2) 0.0843(18) Uani 1 1 d . . . . .
H18A H 0.892544 0.186373 0.593407 0.101 Uiso 1 1 calc R U . . .
H18B H 0.945651 0.162687 0.554702 0.101 Uiso 1 1 calc R U . . .
C20 C 0.7663(4) -0.0127(4) 0.5935(2) 0.0889(19) Uani 1 1 d . . . . .
H20A H 0.724741 -0.014468 0.614302 0.107 Uiso 1 1 calc R U . . .
H20B H 0.806740 -0.047562 0.603005 0.107 Uiso 1 1 calc R U . . .
C22 C 0.7370(4) -0.0381(4) 0.5508(2) 0.090(2) Uani 1 1 d . . . . .
H22A H 0.710106 -0.087061 0.553553 0.109 Uiso 1 1 calc R U . . .
H22B H 0.779703 -0.044883 0.531105 0.109 Uiso 1 1 calc R U . . .
C26 C 0.8793(4) 0.0730(4) 0.5764(2) 0.0887(19) Uani 1 1 d . . . . .
H26A H 0.887545 0.042199 0.550820 0.106 Uiso 1 1 calc R U . . .
H26B H 0.913774 0.054641 0.598620 0.106 Uiso 1 1 calc R U . . .
O11 O 0.5659(6) 0.0261(4) 0.6032(3) 0.056(2) Uani 0.5 1 d . . P . .
O13 O 0.4366(7) -0.0222(7) 0.6061(3) 0.068(3) Uani 0.5 1 d . . P . .
O12 O 0.5184(10) -0.0583(10) 0.5512(5) 0.068(4) Uani 0.5 1 d . . P . .
O15 O 0.5450(6) -0.1017(5) 0.6211(3) 0.090(3) Uani 0.5 1 d . . P . .
O14 O 0.5814(8) -0.0295(14) 0.6148(4) 0.198(10) Uani 0.5 1 d . . P . .
O16 O 0.5291(8) -0.1428(5) 0.5873(3) 0.120(4) Uani 0.5 1 d . . P . .
O17 O 0.5155(14) -0.0322(12) 0.5528(6) 0.118(8) Uani 0.5 1 d . . P . .
O18 O 0.4552(8) -0.0488(8) 0.6211(4) 0.082(3) Uani 0.5 1 d . . P . .
O21 O 0.8926(6) 0.4640(6) 0.5158(4) 0.094(3) Uani 0.5 1 d . . P . .
O22 O 0.8094(5) 0.3751(7) 0.5487(3) 0.088(3) Uani 0.5 1 d . . P . .
O23 O 0.9234(5) 0.4155(8) 0.5830(3) 0.107(3) Uani 0.5 1 d . . P . .
O24 O 0.9319(5) 0.3381(5) 0.5230(3) 0.090(2) Uani 0.5 1 d . . P . .
O25 O 0.9105(4) 0.3466(5) 0.5773(2) 0.0648(18) Uani 0.5 1 d . . P . .
O26 O 0.8227(7) 0.3552(6) 0.5221(4) 0.104(4) Uani 0.5 1 d . . P . .
O27 O 0.9394(9) 0.4238(8) 0.5178(3) 0.134(5) Uani 0.5 1 d . . P . .
O28 O 0.8475(6) 0.4648(5) 0.5651(3) 0.101(3) Uani 0.5 1 d . . P . .
OW O 0.500000 0.250000 0.4186(3) 0.174(4) Uani 1 2 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 N4 2.006(5) . ?
Cu1 N2 2.015(4) . ?
Cu1 N1 2.025(4) . ?
Cu1 N3 2.063(4) . ?
Cu1 N5 2.140(4) . ?
Cl1 O15 1.279(7) . ?
Cl1 O14 1.307(12) . ?
Cl1 O18 1.352(13) . ?
Cl1 O17 1.37(2) . ?
Cl1 O12 1.387(15) . ?
Cl1 O13 1.531(12) . ?
Cl1 O11 1.589(10) . ?
Cl1 O16 1.622(8) . ?
Cl2 O22 1.345(10) . ?
Cl2 O27 1.363(11) . ?
Cl2 O23 1.411(8) . ?
Cl2 O25 1.434(7) . ?
Cl2 O28 1.451(8) . ?
Cl2 O21 1.463(10) . ?
Cl2 O26 1.470(9) . ?
Cl2 O24 1.505(9) . ?
N3 C11 1.473(7) . ?
N3 C12 1.475(6) . ?
N3 C16 1.492(7) . ?
N2 C14 1.476(6) . ?
N2 C18 1.477(7) . ?
N5 C31 1.316(6) . ?
N5 C4 1.387(5) . ?
C4 C7 1.399(6) . ?
C4 C29 1.404(7) . ?
C31 C6 1.406(7) . ?
C31 C11 1.519(7) . ?
N4 C17 1.471(8) . ?
N4 C22 1.492(8) . ?
C30 C6 1.361(8) . ?
C30 C29 1.414(7) . ?
C7 C13 1.371(7) . ?
C29 C10 1.423(7) . ?
N1 C20 1.477(8) . ?
N1 C26 1.495(7) . ?
C10 C15 1.353(8) . ?
C12 C14 1.508(7) . ?
C13 C15 1.384(8) . ?
C16 C17 1.539(8) . ?
C18 C26 1.501(9) . ?
C20 C22 1.491(9) . ?
O11 O14 1.06(3) . ?
O13 O18 0.731(11) . ?
O15 O16 1.302(12) . ?
O15 O14 1.41(2) . ?
O15 O18 1.805(16) . ?
O21 O27 1.069(14) . ?
O21 O28 1.727(15) . ?
O22 O26 0.930(12) . ?
O22 O28 1.765(15) . ?
O23 O25 1.226(12) . ?
O23 O28 1.663(13) . ?
O24 O27 1.499(15) . ?
O24 O25 1.743(11) . ?

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
N4 Cu1 N2 147.38(18) . . ?
N4 Cu1 N1 86.1(2) . . ?
N2 Cu1 N1 85.19(19) . . ?
N4 Cu1 N3 86.96(18) . . ?
N2 Cu1 N3 86.10(16) . . ?
N1 Cu1 N3 151.80(18) . . ?
N4 Cu1 N5 108.06(18) . . ?
N2 Cu1 N5 102.28(16) . . ?
N1 Cu1 N5 126.92(16) . . ?
N3 Cu1 N5 81.17(15) . . ?
O15 Cl1 O14 66.3(11) . . ?
O15 Cl1 O18 86.6(7) . . ?
O14 Cl1 O18 113.1(8) . . ?
O15 Cl1 O17 141.6(10) . . ?
O14 Cl1 O17 114.1(12) . . ?
O18 Cl1 O17 123.0(11) . . ?
O15 Cl1 O12 124.0(8) . . ?
O14 Cl1 O12 118.9(9) . . ?
O18 Cl1 O12 126.7(9) . . ?
O17 Cl1 O12 19.1(14) . . ?
O15 Cl1 O13 115.0(6) . . ?
O14 Cl1 O13 125.3(9) . . ?
O18 Cl1 O13 28.5(5) . . ?
O17 Cl1 O13 96.1(10) . . ?
O12 Cl1 O13 104.6(8) . . ?
O15 Cl1 O11 106.8(6) . . ?
O14 Cl1 O11 41.6(12) . . ?
O18 Cl1 O11 107.8(7) . . ?
O17 Cl1 O11 88.0(10) . . ?
O12 Cl1 O11 103.1(8) . . ?
O13 Cl1 O11 100.0(6) . . ?
O15 Cl1 O16 51.7(5) . . ?
O14 Cl1 O16 104.6(12) . . ?
O18 Cl1 O16 102.4(7) . . ?
O17 Cl1 O16 94.9(9) . . ?
O12 Cl1 O16 75.7(8) . . ?
O13 Cl1 O16 117.6(7) . . ?
O11 Cl1 O16 141.7(6) . . ?
O22 Cl2 O27 146.3(8) . . ?
O22 Cl2 O23 117.1(6) . . ?
O27 Cl2 O23 95.8(8) . . ?
O22 Cl2 O25 93.6(5) . . ?
O27 Cl2 O25 113.8(7) . . ?
O23 Cl2 O25 51.0(5) . . ?
O22 Cl2 O28 78.2(7) . . ?
O27 Cl2 O28 108.5(7) . . ?
O23 Cl2 O28 71.0(6) . . ?
O25 Cl2 O28 109.1(5) . . ?
O22 Cl2 O21 113.3(6) . . ?
O27 Cl2 O21 44.3(6) . . ?
O23 Cl2 O21 107.7(7) . . ?
O25 Cl2 O21 152.4(5) . . ?
O28 Cl2 O21 72.7(6) . . ?
O22 Cl2 O26 38.3(5) . . ?
O27 Cl2 O26 112.0(8) . . ?
O23 Cl2 O26 150.1(7) . . ?
O25 Cl2 O26 105.1(5) . . ?
O28 Cl2 O26 108.2(6) . . ?
O21 Cl2 O26 100.1(6) . . ?
O22 Cl2 O24 111.4(6) . . ?
O27 Cl2 O24 62.8(7) . . ?
O23 Cl2 O24 104.5(5) . . ?
O25 Cl2 O24 72.7(5) . . ?
O28 Cl2 O24 170.3(6) . . ?
O21 Cl2 O24 101.2(6) . . ?
O26 Cl2 O24 80.0(6) . . ?
C11 N3 C12 111.3(4) . . ?
C11 N3 C16 112.5(4) . . ?
C12 N3 C16 112.9(4) . . ?
C11 N3 Cu1 110.7(3) . . ?
C12 N3 Cu1 106.1(3) . . ?
C16 N3 Cu1 102.7(3) . . ?
C14 N2 C18 114.6(4) . . ?
C14 N2 Cu1 101.9(3) . . ?
C18 N2 Cu1 109.2(4) . . ?
C31 N5 C4 119.2(4) . . ?
C31 N5 Cu1 113.0(3) . . ?
C4 N5 Cu1 127.1(3) . . ?
N5 C4 C7 119.2(4) . . ?
N5 C4 C29 121.3(4) . . ?
C7 C4 C29 119.4(4) . . ?
N5 C31 C6 122.1(5) . . ?
N5 C31 C11 116.8(5) . . ?
C6 C31 C11 121.0(4) . . ?
C17 N4 C22 116.2(5) . . ?
C17 N4 Cu1 109.5(4) . . ?
C22 N4 Cu1 105.1(4) . . ?
C6 C30 C29 119.4(5) . . ?
C30 C6 C31 120.1(5) . . ?
C13 C7 C4 120.4(5) . . ?
C4 C29 C30 117.8(5) . . ?
C4 C29 C10 118.1(5) . . ?
C30 C29 C10 124.1(5) . . ?
C20 N1 C26 115.4(5) . . ?
C20 N1 Cu1 107.9(4) . . ?
C26 N1 Cu1 103.3(3) . . ?
C15 C10 C29 121.4(5) . . ?
N3 C11 C31 111.9(4) . . ?
N3 C12 C14 109.8(4) . . ?
C7 C13 C15 121.0(5) . . ?
N2 C14 C12 107.8(4) . . ?
C10 C15 C13 119.8(5) . . ?
N3 C16 C17 110.1(4) . . ?
N4 C17 C16 110.9(5) . . ?
N2 C18 C26 108.8(5) . . ?
N1 C20 C22 110.2(5) . . ?
C20 C22 N4 108.2(5) . . ?
N1 C26 C18 107.3(5) . . ?
O14 O11 Cl1 54.8(9) . . ?
O18 O13 Cl1 62.0(17) . . ?
Cl1 O15 O16 77.8(6) . . ?
Cl1 O15 O14 57.8(8) . . ?
O16 O15 O14 117.7(9) . . ?
Cl1 O15 O18 48.4(5) . . ?
O16 O15 O18 95.4(9) . . ?
O14 O15 O18 86.3(10) . . ?
O11 O14 Cl1 83.5(16) . . ?
O11 O14 O15 137.4(17) . . ?
Cl1 O14 O15 55.9(6) . . ?
O15 O16 Cl1 50.4(4) . . ?
O13 O18 Cl1 89.5(19) . . ?
O13 O18 O15 134(2) . . ?
Cl1 O18 O15 45.0(5) . . ?
O27 O21 Cl2 62.9(8) . . ?
O27 O21 O28 107.2(10) . . ?
Cl2 O21 O28 53.3(5) . . ?
O26 O22 Cl2 78.2(11) . . ?
O26 O22 O28 119.5(13) . . ?
Cl2 O22 O28 53.6(5) . . ?
O25 O23 Cl2 65.4(5) . . ?
O25 O23 O28 107.9(8) . . ?
Cl2 O23 O28 55.6(4) . . ?
O27 O24 Cl2 53.9(5) . . ?
O27 O24 O25 92.3(6) . . ?
Cl2 O24 O25 51.8(4) . . ?
O23 O25 Cl2 63.5(5) . . ?
O23 O25 O24 100.6(7) . . ?
Cl2 O25 O24 55.5(4) . . ?
O22 O26 Cl2 63.6(8) . . ?
O21 O27 Cl2 72.9(10) . . ?
O21 O27 O24 125.7(14) . . ?
Cl2 O27 O24 63.3(6) . . ?
Cl2 O28 O23 53.4(4) . . ?
Cl2 O28 O21 54.0(4) . . ?
O23 O28 O21 86.4(6) . . ?
Cl2 O28 O22 48.2(4) . . ?
O23 O28 O22 86.6(7) . . ?
O21 O28 O22 84.4(5) . . ?

_refine_diff_density_max         0.371
_refine_diff_density_min         -0.675
_refine_diff_density_rms         0.068



# start Validation Reply Form
_vrf_PLAT430_shelx               
;
PROBLEM: Short Inter D...A Contact Ow ..O16 . 1.93 Ang.
RESPONSE: one ofthe atoms involved in this short contact is a water oxygen and the contact can be interpreted
;
_vrf_PLAT306_shelx               
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... Ow Check
RESPONSE: the atom is a water oxygen. Linked hydrogens were not localized in the Fourier difference map
;
# end Validation Reply Form

#===END
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Ca_2ZnL5-ClO4-14H2O
_database_code_depnum_ccdc_archive 'CCDC 2375281'
loop_
_audit_author_name
_audit_author_address
'Patrizia Rossi'
;University of Firenze
Italy
;
_audit_update_record             
;
2024-08-02 deposited with the CCDC.	2024-12-11 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT910_Ca_2ZnL5-ClO4-14H2O 
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min). 67 Note
RESPONSE: this is probably due to the beamstop mask
;
_vrf_PLAT417_Ca_2ZnL5-ClO4-14H2O 
;
PROBLEM: Short Inter D-H..H-D H10W ..H12Y . 2.03 Ang.
RESPONSE: H12Y is involved in a strong hydrogen bond
with the oxygen atom O10W (to which H10w is bonded)
;
# end Validation Reply Form

_publ_section_title_             
;
Zn(II)/Cd(II) selective binding and fluorescence sensing 
by using macrocyclic tetra-amines with different fluorophores. 
Clues for design of selective chemosensors for transition metals.
;


_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C64 H98 Ca Cl2 N12 O30 Zn2'
_chemical_formula_weight         1757.26

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.3537(3)
_cell_length_b                   16.8712(4)
_cell_length_c                   19.1547(4)
_cell_angle_alpha                83.534(2)
_cell_angle_beta                 83.991(2)
_cell_angle_gamma                81.834(2)
_cell_volume                     3910.64(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    23663
_cell_measurement_theta_min      4.1121
_cell_measurement_theta_max      32.7174

_exptl_crystal_description       prism
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_F_000             1840
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_exptl_absorpt_coefficient_mu    0.837
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.94599
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            87922
_diffrn_reflns_av_unetI/netI     0.0680
_diffrn_reflns_av_R_equivalents  0.0580
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         4.120
_diffrn_reflns_theta_max         32.792
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.903
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.903
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.903
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             26182
_reflns_number_gt                18329
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_cell_refinement       
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_data_reduction        
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_structure_solution    'SIR2004 (Burla, 2005)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Mercury 3.10.1'
_computing_publication_material  'PARST(Nardelli, 1995)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0572P)²+3.6130P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         26182
_refine_ls_number_parameters     1081
_refine_ls_number_restraints     40
_refine_ls_R_factor_all          0.0909
_refine_ls_R_factor_gt           0.0565
_refine_ls_wR_factor_ref         0.1460
_refine_ls_wR_factor_gt          0.1275
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.024
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000

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
Ca1 Ca 1.05835(4) 0.12138(3) 0.31471(2) 0.01858(9) Uani 1 1 d . . . . .
Zn1A Zn 1.26333(2) -0.11165(2) 0.27233(2) 0.01776(6) Uani 1 1 d . . . . .
O1A O 1.14534(14) -0.02598(10) 0.31079(9) 0.0205(3) Uani 1 1 d . . . . .
O2A O 0.98776(14) -0.00414(10) 0.37461(9) 0.0233(4) Uani 1 1 d . . . . .
O3A O 1.33963(14) -0.02373(10) 0.21486(9) 0.0242(4) Uani 1 1 d . . . . .
O4A O 1.48136(18) -0.00197(13) 0.13637(12) 0.0409(5) Uani 1 1 d . . . . .
N1A N 1.15760(17) -0.19207(12) 0.33412(11) 0.0209(4) Uani 1 1 d . . . . .
N2A N 1.36032(17) -0.14246(12) 0.36691(11) 0.0201(4) Uani 1 1 d . . . . .
N3A N 1.39991(17) -0.18893(12) 0.22425(11) 0.0208(4) Uani 1 1 d . . . . .
N4A N 1.17698(17) -0.14441(12) 0.18526(11) 0.0216(4) Uani 1 1 d . . . . .
N5A N 1.37029(18) -0.07273(13) 0.52143(11) 0.0245(4) Uani 1 1 d . . . . .
N6A N 0.94385(17) -0.08310(13) 0.10872(11) 0.0222(4) Uani 1 1 d . . . . .
C1A C 1.2200(2) -0.23761(14) 0.39080(13) 0.0225(5) Uani 1 1 d . . . . .
H1A1 H 1.269149 -0.283266 0.371719 0.027 Uiso 1 1 calc R U . . .
H1A2 H 1.168411 -0.259692 0.428662 0.027 Uiso 1 1 calc R U . . .
C2A C 1.2874(2) -0.18355(15) 0.42101(13) 0.0238(5) Uani 1 1 d . . . . .
H2A1 H 1.237151 -0.142499 0.445742 0.029 Uiso 1 1 calc R U . . .
H2A2 H 1.332680 -0.216247 0.456264 0.029 Uiso 1 1 calc R U . . .
C3A C 1.4616(2) -0.19535(16) 0.34378(14) 0.0249(5) Uani 1 1 d . . . . .
H3A1 H 1.483443 -0.234101 0.384229 0.030 Uiso 1 1 calc R U . . .
H3A2 H 1.521461 -0.161818 0.330280 0.030 Uiso 1 1 calc R U . . .
C4A C 1.4499(2) -0.24214(15) 0.28209(13) 0.0231(5) Uani 1 1 d . . . . .
H4A1 H 1.523142 -0.267950 0.264464 0.028 Uiso 1 1 calc R U . . .
H4A2 H 1.403575 -0.285129 0.298380 0.028 Uiso 1 1 calc R U . . .
C5A C 1.3555(2) -0.23388(17) 0.17439(14) 0.0289(6) Uani 1 1 d . . . . .
H5A1 H 1.325301 -0.281133 0.200461 0.035 Uiso 1 1 calc R U . . .
H5A2 H 1.415439 -0.253641 0.139601 0.035 Uiso 1 1 calc R U . . .
C6A C 1.2661(2) -0.18109(17) 0.13612(14) 0.0287(6) Uani 1 1 d . . . . .
H6A1 H 1.298754 -0.137786 0.105393 0.034 Uiso 1 1 calc R U . . .
H6A2 H 1.234512 -0.213772 0.105571 0.034 Uiso 1 1 calc R U . . .
C7A C 1.0982(2) -0.19996(17) 0.21593(15) 0.0301(6) Uani 1 1 d . . . . .
H7A1 H 1.093359 -0.238762 0.181623 0.036 Uiso 1 1 calc R U . . .
H7A2 H 1.024632 -0.168663 0.223739 0.036 Uiso 1 1 calc R U . . .
C8A C 1.1291(2) -0.24635(15) 0.28524(14) 0.0264(5) Uani 1 1 d . . . . .
H8A1 H 1.066746 -0.273950 0.307494 0.032 Uiso 1 1 calc R U . . .
H8A2 H 1.192536 -0.287895 0.275975 0.032 Uiso 1 1 calc R U . . .
C9A C 1.3882(2) -0.06867(15) 0.39390(13) 0.0221(5) Uani 1 1 d . . . . .
H9A1 H 1.320730 -0.029609 0.399057 0.026 Uiso 1 1 calc R U . . .
H9A2 H 1.440860 -0.043538 0.358688 0.026 Uiso 1 1 calc R U . . .
C10A C 1.4378(2) -0.08556(14) 0.46443(13) 0.0219(5) Uani 1 1 d . . . . .
C11A C 1.5500(2) -0.11604(17) 0.46820(15) 0.0291(6) Uani 1 1 d . . . . .
H11A H 1.596999 -0.123335 0.426247 0.035 Uiso 1 1 calc R U . . .
C12A C 1.5901(2) -0.13487(18) 0.53248(16) 0.0323(6) Uani 1 1 d . . . . .
H12A H 1.664769 -0.156982 0.535534 0.039 Uiso 1 1 calc R U . . .
C13A C 1.5210(2) -0.12156(16) 0.59409(15) 0.0278(5) Uani 1 1 d . . . . .
C14A C 1.5565(3) -0.13756(19) 0.66291(16) 0.0358(7) Uani 1 1 d . . . . .
H14A H 1.630525 -0.159574 0.668776 0.043 Uiso 1 1 calc R U . . .
C15A C 1.4862(3) -0.1219(2) 0.72051(16) 0.0400(7) Uani 1 1 d . . . . .
H15A H 1.511253 -0.133064 0.766269 0.048 Uiso 1 1 calc R U . . .
C16A C 1.3761(3) -0.0890(2) 0.71271(16) 0.0410(7) Uani 1 1 d . . . . .
H16A H 1.327601 -0.077612 0.753258 0.049 Uiso 1 1 calc R U . . .
C17A C 1.3386(3) -0.0733(2) 0.64704(15) 0.0360(7) Uani 1 1 d . . . . .
H17A H 1.264149 -0.051496 0.642316 0.043 Uiso 1 1 calc R U . . .
C18A C 1.4100(2) -0.08927(16) 0.58660(14) 0.0253(5) Uani 1 1 d . . . . .
C19A C 1.1181(2) -0.07026(14) 0.14958(13) 0.0211(5) Uani 1 1 d . . . . .
H19A H 1.172856 -0.034570 0.129157 0.025 Uiso 1 1 calc R U . . .
H19B H 1.069094 -0.041623 0.185577 0.025 Uiso 1 1 calc R U . . .
C20A C 1.0504(2) -0.08392(14) 0.09179(13) 0.0203(4) Uani 1 1 d . . . . .
C21A C 1.0996(2) -0.09475(15) 0.02278(13) 0.0223(5) Uani 1 1 d . . . . .
H21A H 1.176459 -0.094658 0.012314 0.027 Uiso 1 1 calc R U . . .
C22A C 1.0360(2) -0.10530(15) -0.02846(13) 0.0228(5) Uani 1 1 d . . . . .
H22A H 1.068226 -0.113096 -0.074854 0.027 Uiso 1 1 calc R U . . .
C23A C 0.9217(2) -0.10455(14) -0.01201(13) 0.0220(5) Uani 1 1 d . . . . .
C24A C 0.8494(2) -0.11175(16) -0.06277(14) 0.0264(5) Uani 1 1 d . . . . .
H24A H 0.877900 -0.121537 -0.109481 0.032 Uiso 1 1 calc R U . . .
C25A C 0.7393(2) -0.10472(19) -0.04502(16) 0.0335(6) Uani 1 1 d . . . . .
H25A H 0.691287 -0.109251 -0.079599 0.040 Uiso 1 1 calc R U . . .
C26A C 0.6954(2) -0.0907(2) 0.02431(16) 0.0389(7) Uani 1 1 d . . . . .
H26A H 0.618143 -0.084960 0.035801 0.047 Uiso 1 1 calc R U . . .
C27A C 0.7636(2) -0.08549(19) 0.07492(15) 0.0337(6) Uani 1 1 d . . . . .
H27A H 0.733741 -0.077283 0.121705 0.040 Uiso 1 1 calc R U . . .
C28A C 0.8783(2) -0.09222(15) 0.05789(13) 0.0223(5) Uani 1 1 d . . . . .
C29A C 1.0596(2) -0.14076(15) 0.36341(15) 0.0275(5) Uani 1 1 d . . . . .
H29A H 1.050072 -0.154840 0.415073 0.033 Uiso 1 1 calc R U . . .
H29B H 0.994094 -0.153333 0.343364 0.033 Uiso 1 1 calc R U . . .
C30A C 1.06442(19) -0.05115(14) 0.34919(12) 0.0194(4) Uani 1 1 d . . . . .
C31A C 1.4759(2) -0.13465(16) 0.18690(14) 0.0272(5) Uani 1 1 d . . . . .
H31A H 1.499774 -0.152612 0.139596 0.033 Uiso 1 1 calc R U . . .
H31B H 1.541995 -0.140071 0.213082 0.033 Uiso 1 1 calc R U . . .
C32A C 1.4285(2) -0.04599(16) 0.17796(13) 0.0248(5) Uani 1 1 d . . . . .
Zn1B Zn 0.84637(2) 0.32622(2) 0.19546(2) 0.01862(6) Uani 1 1 d . . . . .
O1B O 0.96908(14) 0.25671(10) 0.25338(9) 0.0215(3) Uani 1 1 d . . . . .
O2B O 1.11070(15) 0.25811(10) 0.31417(9) 0.0243(4) Uani 1 1 d . . . . .
O3B O 0.81523(14) 0.22040(10) 0.16968(9) 0.0236(4) Uani 1 1 d . . . . .
O4B O 0.71758(16) 0.15462(11) 0.11037(11) 0.0317(4) Uani 1 1 d . . . . .
N1B N 0.93090(17) 0.41814(12) 0.23080(11) 0.0204(4) Uani 1 1 d . . . . .
N2B N 0.71889(17) 0.36744(12) 0.27625(11) 0.0216(4) Uani 1 1 d . . . . .
N3B N 0.70276(17) 0.36851(12) 0.12807(11) 0.0221(4) Uani 1 1 d . . . . .
N4B N 0.93617(17) 0.36775(12) 0.09346(11) 0.0210(4) Uani 1 1 d . . . . .
N5B N 0.70448(18) 0.37175(13) 0.44851(11) 0.0235(4) Uani 1 1 d . . . . .
N6B N 1.20026(18) 0.33381(13) 0.03104(12) 0.0263(4) Uani 1 1 d . . . . .
C1B C 0.8646(2) 0.44826(15) 0.29354(13) 0.0241(5) Uani 1 1 d . . . . .
H1B1 H 0.878583 0.503760 0.297864 0.029 Uiso 1 1 calc R U . . .
H1B2 H 0.887345 0.414074 0.336354 0.029 Uiso 1 1 calc R U . . .
C2B C 0.7432(2) 0.44805(15) 0.28909(14) 0.0251(5) Uani 1 1 d . . . . .
H2B1 H 0.702238 0.463868 0.333710 0.030 Uiso 1 1 calc R U . . .
H2B2 H 0.718054 0.488152 0.250357 0.030 Uiso 1 1 calc R U . . .
C3B C 0.6107(2) 0.37310(16) 0.24742(14) 0.0256(5) Uani 1 1 d . . . . .
H3B1 H 0.554273 0.404937 0.277240 0.031 Uiso 1 1 calc R U . . .
H3B2 H 0.589540 0.318480 0.248648 0.031 Uiso 1 1 calc R U . . .
C4B C 0.6147(2) 0.41247(16) 0.17217(14) 0.0259(5) Uani 1 1 d . . . . .
H4B1 H 0.543288 0.412456 0.153043 0.031 Uiso 1 1 calc R U . . .
H4B2 H 0.628163 0.469037 0.171390 0.031 Uiso 1 1 calc R U . . .
C5B C 0.7459(2) 0.41937(16) 0.06681(13) 0.0248(5) Uani 1 1 d . . . . .
H5B1 H 0.752631 0.472999 0.080956 0.030 Uiso 1 1 calc R U . . .
H5B2 H 0.694697 0.426752 0.029475 0.030 Uiso 1 1 calc R U . . .
C6B C 0.8574(2) 0.37986(17) 0.03873(13) 0.0258(5) Uani 1 1 d . . . . .
H6B1 H 0.849706 0.327208 0.022921 0.031 Uiso 1 1 calc R U . . .
H6B2 H 0.886053 0.414056 -0.002540 0.031 Uiso 1 1 calc R U . . .
C7B C 0.9809(2) 0.44297(15) 0.10233(13) 0.0245(5) Uani 1 1 d . . . . .
H7B1 H 0.964783 0.482750 0.061438 0.029 Uiso 1 1 calc R U . . .
H7B2 H 1.061739 0.431109 0.102446 0.029 Uiso 1 1 calc R U . . .
C8B C 0.9341(2) 0.48001(15) 0.16989(13) 0.0232(5) Uani 1 1 d . . . . .
H8B1 H 0.979876 0.520716 0.179017 0.028 Uiso 1 1 calc R U . . .
H8B2 H 0.858889 0.507559 0.163931 0.028 Uiso 1 1 calc R U . . .
C9B C 0.7257(2) 0.30844(15) 0.34048(13) 0.0232(5) Uani 1 1 d . . . . .
H9B1 H 0.803113 0.297080 0.351709 0.028 Uiso 1 1 calc R U . . .
H9B2 H 0.703419 0.257408 0.329568 0.028 Uiso 1 1 calc R U . . .
C10B C 0.6553(2) 0.33595(15) 0.40511(13) 0.0236(5) Uani 1 1 d . . . . .
C11B C 0.5434(2) 0.32407(16) 0.41707(15) 0.0278(5) Uani 1 1 d . . . . .
H11B H 0.510938 0.297856 0.384774 0.033 Uiso 1 1 calc R U . . .
C12B C 0.4826(2) 0.35079(17) 0.47565(16) 0.0319(6) Uani 1 1 d . . . . .
H12B H 0.407470 0.343248 0.484373 0.038 Uiso 1 1 calc R U . . .
C13B C 0.5319(2) 0.38962(16) 0.52312(14) 0.0279(5) Uani 1 1 d . . . . .
C14B C 0.4772(3) 0.41668(18) 0.58675(16) 0.0369(7) Uani 1 1 d . . . . .
H14B H 0.401805 0.411062 0.598323 0.044 Uiso 1 1 calc R U . . .
C15B C 0.5314(3) 0.45031(18) 0.63093(16) 0.0393(7) Uani 1 1 d . . . . .
H15B H 0.493972 0.466554 0.673941 0.047 Uiso 1 1 calc R U . . .
C16B C 0.6416(3) 0.46175(18) 0.61471(16) 0.0366(7) Uani 1 1 d . . . . .
H16B H 0.677811 0.486378 0.646185 0.044 Uiso 1 1 calc R U . . .
C17B C 0.6972(3) 0.43736(17) 0.55326(15) 0.0320(6) Uani 1 1 d . . . . .
H17B H 0.771580 0.446134 0.541818 0.038 Uiso 1 1 calc R U . . .
C18B C 0.6443(2) 0.39936(15) 0.50717(14) 0.0255(5) Uani 1 1 d . . . . .
C19B C 1.0245(2) 0.29936(15) 0.08007(13) 0.0227(5) Uani 1 1 d . . . . .
H19C H 0.989326 0.251750 0.073814 0.027 Uiso 1 1 calc R U . . .
H19D H 1.065495 0.285975 0.122495 0.027 Uiso 1 1 calc R U . . .
C20B C 1.1055(2) 0.31400(15) 0.01704(13) 0.0241(5) Uani 1 1 d . . . . .
C21B C 1.0809(2) 0.30576(16) -0.05169(14) 0.0283(5) Uani 1 1 d . . . . .
H21B H 1.011830 0.291295 -0.059388 0.034 Uiso 1 1 calc R U . . .
C22B C 1.1571(3) 0.31873(17) -0.10701(15) 0.0340(6) Uani 1 1 d . . . . .
H22B H 1.142264 0.311863 -0.153478 0.041 Uiso 1 1 calc R U . . .
C23B C 1.2575(3) 0.34228(16) -0.09512(15) 0.0329(6) Uani 1 1 d . . . . .
C24B C 1.3404(3) 0.35868(18) -0.14927(19) 0.0444(8) Uani 1 1 d . . . . .
H24B H 1.329233 0.353699 -0.196824 0.053 Uiso 1 1 calc R U . . .
C25B C 1.4356(3) 0.38144(19) -0.1343(2) 0.0512(10) Uani 1 1 d . . . . .
H25B H 1.490196 0.392720 -0.171436 0.061 Uiso 1 1 calc R U . . .
C26B C 1.4540(3) 0.38844(19) -0.0643(2) 0.0494(10) Uani 1 1 d . . . . .
H26B H 1.521315 0.404202 -0.054518 0.059 Uiso 1 1 calc R U . . .
C27B C 1.3762(2) 0.37284(19) -0.0097(2) 0.0405(7) Uani 1 1 d . . . . .
H27B H 1.389502 0.377770 0.037491 0.049 Uiso 1 1 calc R U . . .
C28B C 1.2765(2) 0.34943(15) -0.02432(15) 0.0290(6) Uani 1 1 d . . . . .
C29B C 1.0416(2) 0.38171(15) 0.25015(14) 0.0243(5) Uani 1 1 d . . . . .
C30B C 1.0405(2) 0.29320(15) 0.27541(12) 0.0206(4) Uani 1 1 d . . . . .
C31B C 0.6677(2) 0.29501(16) 0.10767(15) 0.0271(5) Uani 1 1 d . . . . .
H31C H 0.667378 0.300013 0.055697 0.032 Uiso 1 1 calc R U . . .
H31D H 0.591381 0.291668 0.128181 0.032 Uiso 1 1 calc R U . . .
C32B C 0.7389(2) 0.21646(15) 0.13056(13) 0.0214(5) Uani 1 1 d . . . . .
Cl1 Cl 1.23356(6) 0.56918(5) 0.15732(4) 0.03700(16) Uani 1 1 d . . . . .
O10 O 1.3153(3) 0.5561(2) 0.20578(15) 0.0735(9) Uani 1 1 d . . . . .
O11 O 1.2232(2) 0.49588(15) 0.13000(16) 0.0583(7) Uani 1 1 d . . . . .
O12 O 1.2633(2) 0.62742(15) 0.10151(13) 0.0521(7) Uani 1 1 d . . . . .
O13 O 1.1313(3) 0.59854(19) 0.19367(19) 0.0769(10) Uani 1 1 d . . . . .
Cl2 Cl 1.77329(7) -0.25664(8) 0.31411(6) 0.0613(3) Uani 1 1 d . . . . .
O21A O 1.8016(5) -0.1929(4) 0.3536(3) 0.0700(19) Uiso 0.524(6) 1 d . . P A 1
O22A O 1.7227(4) -0.2093(3) 0.2515(3) 0.0475(13) Uiso 0.524(6) 1 d . . P A 1
O23A O 1.8761(5) -0.2949(4) 0.2814(3) 0.0595(16) Uiso 0.524(6) 1 d . . P A 1
O24A O 1.7063(5) -0.3005(3) 0.3498(3) 0.0576(16) Uiso 0.524(6) 1 d . . P A 1
O21B O 1.7254(6) -0.3358(4) 0.3030(4) 0.075(2) Uiso 0.476(6) 1 d . . P A 2
O22B O 1.7332(6) -0.2687(4) 0.3942(4) 0.079(2) Uiso 0.476(6) 1 d . . P A 2
O23B O 1.7148(7) -0.1915(5) 0.2809(5) 0.080(2) Uiso 0.476(6) 1 d . . P A 2
O24B O 1.8830(9) -0.2749(7) 0.3101(6) 0.113(4) Uiso 0.476(6) 1 d . . P A 2
O1W O 0.85448(16) 0.03344(12) 0.49034(10) 0.0264(4) Uani 1 1 d D . . . .
H1W1 H 0.886(2) 0.0124(18) 0.4551(13) 0.032 Uiso 1 1 d D U . . .
H1W2 H 0.7878(15) 0.0410(19) 0.4838(16) 0.032 Uiso 1 1 d D U . . .
O2W O 1.21272(16) 0.12381(11) 0.22986(10) 0.0263(4) Uani 1 1 d D . . . .
H2W1 H 1.243(2) 0.1609(14) 0.2091(16) 0.032 Uiso 1 1 d D U . . .
H2W2 H 1.257(2) 0.0817(13) 0.2207(16) 0.032 Uiso 1 1 d D U . . .
O3W O 0.92196(16) 0.17249(11) 0.40478(10) 0.0268(4) Uani 1 1 d D . . . .
H3W1 H 0.930(3) 0.2142(13) 0.4235(15) 0.032 Uiso 1 1 d D U . . .
H3W2 H 0.904(3) 0.1397(15) 0.4383(13) 0.032 Uiso 1 1 d D U . . .
O4W O 1.16346(16) 0.10105(12) 0.41334(10) 0.0264(4) Uani 1 1 d D . . . .
H4W1 H 1.154(3) 0.1398(14) 0.4378(15) 0.032 Uiso 1 1 d D U . . .
H4W2 H 1.151(3) 0.0598(13) 0.4378(15) 0.032 Uiso 1 1 d D U . . .
O5W O 0.93846(16) 0.09043(11) 0.23737(11) 0.0296(4) Uani 1 1 d D . . . .
H5W1 H 0.901(2) 0.1297(14) 0.2181(16) 0.036 Uiso 1 1 d D U . . .
H5W2 H 0.903(2) 0.0510(14) 0.2425(18) 0.036 Uiso 1 1 d D U . . .
O6W O 0.93654(18) 0.32221(13) 0.45357(12) 0.0351(5) Uani 1 1 d D . . . .
H6W1 H 0.8715(16) 0.3449(19) 0.4518(19) 0.042 Uiso 1 1 d D U . . .
H6W2 H 0.978(2) 0.3558(17) 0.4447(19) 0.042 Uiso 1 1 d D U . . .
O7W O 1.32056(19) 0.25127(14) 0.15113(11) 0.0383(5) Uani 1 1 d D . . . .
H7W1 H 1.285(3) 0.275(2) 0.1181(15) 0.046 Uiso 1 1 d D U . . .
H7W2 H 1.377(2) 0.224(2) 0.1307(17) 0.046 Uiso 1 1 d D U . . .
O8W O 0.8552(2) -0.05183(14) 0.24480(11) 0.0388(5) Uani 1 1 d D . . . .
H8W1 H 0.818(3) -0.0878(18) 0.2634(17) 0.047 Uiso 1 1 d D U . . .
H8W2 H 0.867(3) -0.061(2) 0.2018(10) 0.047 Uiso 1 1 d D U . . .
O9W O 1.49617(18) 0.15566(14) 0.09162(14) 0.0425(5) Uani 1 1 d D . . . .
H9W1 H 1.491(3) 0.1059(12) 0.103(2) 0.051 Uiso 1 1 d D U . . .
H9W2 H 1.5634(17) 0.160(2) 0.095(2) 0.051 Uiso 1 1 d D U . . .
O10W O 1.2715(2) 0.32745(19) 0.37145(15) 0.0555(7) Uani 1 1 d D . . . .
H10W H 1.223(3) 0.301(2) 0.362(2) 0.067 Uiso 1 1 d D U . . .
H10Y H 1.299(3) 0.349(2) 0.3340(15) 0.067 Uiso 1 1 d D U . . .
O11W O 1.1277(2) 0.21933(16) 0.50555(14) 0.0492(6) Uani 1 1 d D . . . .
H11W H 1.075(2) 0.254(2) 0.497(2) 0.059 Uiso 1 1 d D U . . .
H11Y H 1.160(3) 0.225(2) 0.5388(16) 0.059 Uiso 1 1 d D U . . .
O12W O 1.1033(2) 0.42010(16) 0.43812(15) 0.0522(6) Uani 1 1 d D . . . .
H12W H 1.093(3) 0.4652(15) 0.4140(19) 0.063 Uiso 1 1 d D U . . .
H12Y H 1.164(2) 0.395(2) 0.419(2) 0.063 Uiso 1 1 d D U . . .
O13W O 1.3620(2) 0.36792(16) 0.23421(16) 0.0524(6) Uani 1 1 d D . . . .
H13W H 1.343(3) 0.3334(18) 0.2085(19) 0.063 Uiso 1 1 d D U . . .
H13Y H 1.334(3) 0.4105(15) 0.213(2) 0.063 Uiso 1 1 d D U . . .
O14W O 1.0716(3) 0.5594(2) 0.3529(2) 0.0278(12) Uiso 0.454(6) 1 d . . P B 1
O15W O 1.1350(4) 0.4288(3) 0.5770(2) 0.0358(13) Uiso 0.481(6) 1 d . . P C 2
O16W O 0.9758(17) 0.5747(12) 0.4152(11) 0.011(6) Uiso 0.068(5) 1 d . . P D 3


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Ca1 O5W 2.3483(19) . ?
Ca1 O4W 2.3694(18) . ?
Ca1 O2W 2.3745(19) . ?
Ca1 O3W 2.4234(19) . ?
Ca1 O2B 2.4811(18) . ?
Ca1 O2A 2.5159(18) . ?
Ca1 O1A 2.5705(17) . ?
Ca1 O1B 2.6002(17) . ?
Ca1 C30B 2.895(2) . ?
Ca1 C30A 2.903(2) . ?
Zn1A O3A 2.0280(18) . ?
Zn1A O1A 2.0428(17) . ?
Zn1A N3A 2.171(2) . ?
Zn1A N1A 2.183(2) . ?
Zn1A N4A 2.230(2) . ?
Zn1A N2A 2.248(2) . ?
O1A C30A 1.272(3) . ?
O2A C30A 1.241(3) . ?
O3A C32A 1.275(3) . ?
O4A C32A 1.228(3) . ?
N1A C1A 1.477(3) . ?
N1A C8A 1.481(3) . ?
N1A C29A 1.483(3) . ?
N2A C2A 1.478(3) . ?
N2A C3A 1.488(3) . ?
N2A C9A 1.497(3) . ?
N3A C5A 1.476(3) . ?
N3A C4A 1.475(3) . ?
N3A C31A 1.479(3) . ?
N4A C7A 1.479(3) . ?
N4A C6A 1.484(3) . ?
N4A C19A 1.488(3) . ?
N5A C10A 1.321(3) . ?
N5A C18A 1.374(3) . ?
N6A C20A 1.321(3) . ?
N6A C28A 1.364(3) . ?
C1A C2A 1.516(4) . ?
C3A C4A 1.523(4) . ?
C5A C6A 1.515(4) . ?
C7A C8A 1.519(4) . ?
C9A C10A 1.522(3) . ?
C10A C11A 1.415(3) . ?
C11A C12A 1.363(4) . ?
C12A C13A 1.402(4) . ?
C13A C18A 1.417(4) . ?
C13A C14A 1.418(4) . ?
C14A C15A 1.357(5) . ?
C15A C16A 1.411(5) . ?
C16A C17A 1.371(4) . ?
C17A C18A 1.407(4) . ?
C19A C20A 1.511(3) . ?
C20A C21A 1.416(3) . ?
C21A C22A 1.361(3) . ?
C22A C23A 1.414(4) . ?
C23A C24A 1.413(3) . ?
C23A C28A 1.416(3) . ?
C24A C25A 1.359(4) . ?
C25A C26A 1.413(4) . ?
C26A C27A 1.368(4) . ?
C27A C28A 1.412(4) . ?
C29A C30A 1.514(3) . ?
C31A C32A 1.525(4) . ?
Zn1B O3B 2.0030(17) . ?
Zn1B O1B 2.1114(16) . ?
Zn1B N2B 2.186(2) . ?
Zn1B N1B 2.190(2) . ?
Zn1B N4B 2.236(2) . ?
Zn1B N3B 2.288(2) . ?
O1B C30B 1.275(3) . ?
O2B C30B 1.243(3) . ?
O3B C32B 1.278(3) . ?
O4B C32B 1.224(3) . ?
N1B C8B 1.477(3) . ?
N1B C1B 1.479(3) . ?
N1B C29B 1.484(3) . ?
N2B C2B 1.486(3) . ?
N2B C3B 1.486(3) . ?
N2B C9B 1.495(3) . ?
N3B C4B 1.472(3) . ?
N3B C5B 1.473(3) . ?
N3B C31B 1.474(3) . ?
N4B C6B 1.482(3) . ?
N4B C7B 1.488(3) . ?
N4B C19B 1.496(3) . ?
N5B C10B 1.322(3) . ?
N5B C18B 1.370(3) . ?
N6B C20B 1.323(3) . ?
N6B C28B 1.371(3) . ?
C1B C2B 1.511(4) . ?
C3B C4B 1.517(4) . ?
C5B C6B 1.515(4) . ?
C7B C8B 1.524(4) . ?
C9B C10B 1.514(4) . ?
C10B C11B 1.417(4) . ?
C11B C12B 1.366(4) . ?
C12B C13B 1.411(4) . ?
C13B C18B 1.419(4) . ?
C13B C14B 1.420(4) . ?
C14B C15B 1.349(5) . ?
C15B C16B 1.400(5) . ?
C16B C17B 1.374(4) . ?
C17B C18B 1.409(4) . ?
C19B C20B 1.507(3) . ?
C20B C21B 1.408(4) . ?
C21B C22B 1.361(4) . ?
C22B C23B 1.403(5) . ?
C23B C24B 1.412(4) . ?
C23B C28B 1.421(4) . ?
C24B C25B 1.355(5) . ?
C25B C26B 1.405(6) . ?
C26B C27B 1.373(5) . ?
C27B C28B 1.410(4) . ?
C29B C30B 1.518(3) . ?
C31B C32B 1.530(4) . ?
Cl1 O10 1.420(3) . ?
Cl1 O11 1.423(2) . ?
Cl1 O12 1.424(2) . ?
Cl1 O13 1.429(3) . ?
Cl2 O24A 1.281(6) . ?
Cl2 O24B 1.343(11) . ?
Cl2 O23B 1.359(8) . ?
Cl2 O23A 1.453(6) . ?
Cl2 O21A 1.481(6) . ?
Cl2 O22A 1.505(5) . ?
Cl2 O22B 1.562(8) . ?
Cl2 O21B 1.579(7) . ?

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
O5W Ca1 O4W 156.83(7) . . ?
O5W Ca1 O2W 95.59(7) . . ?
O4W Ca1 O2W 94.75(7) . . ?
O5W Ca1 O3W 98.27(7) . . ?
O4W Ca1 O3W 79.62(7) . . ?
O2W Ca1 O3W 156.50(7) . . ?
O5W Ca1 O2B 122.88(6) . . ?
O4W Ca1 O2B 79.81(6) . . ?
O2W Ca1 O2B 75.86(6) . . ?
O3W Ca1 O2B 80.67(7) . . ?
O5W Ca1 O2A 75.78(7) . . ?
O4W Ca1 O2A 81.29(6) . . ?
O2W Ca1 O2A 124.96(6) . . ?
O3W Ca1 O2A 77.08(6) . . ?
O2B Ca1 O2A 153.00(6) . . ?
O5W Ca1 O1A 85.01(6) . . ?
O4W Ca1 O1A 77.95(6) . . ?
O2W Ca1 O1A 74.23(6) . . ?
O3W Ca1 O1A 125.76(6) . . ?
O2B Ca1 O1A 140.74(6) . . ?
O2A Ca1 O1A 51.12(5) . . ?
O5W Ca1 O1B 72.62(6) . . ?
O4W Ca1 O1B 128.16(6) . . ?
O2W Ca1 O1B 89.61(6) . . ?
O3W Ca1 O1B 76.64(6) . . ?
O2B Ca1 O1B 51.37(5) . . ?
O2A Ca1 O1B 134.96(6) . . ?
O1A Ca1 O1B 151.06(6) . . ?
O5W Ca1 C30B 98.06(7) . . ?
O4W Ca1 C30B 103.99(7) . . ?
O2W Ca1 C30B 81.14(7) . . ?
O3W Ca1 C30B 78.20(7) . . ?
O2B Ca1 C30B 25.26(6) . . ?
O2A Ca1 C30B 153.30(6) . . ?
O1A Ca1 C30B 155.36(6) . . ?
O1B Ca1 C30B 26.13(6) . . ?
O5W Ca1 C30A 78.40(7) . . ?
O4W Ca1 C30A 79.42(7) . . ?
O2W Ca1 C30A 99.88(7) . . ?
O3W Ca1 C30A 101.44(7) . . ?
O2B Ca1 C30A 158.36(6) . . ?
O2A Ca1 C30A 25.19(6) . . ?
O1A Ca1 C30A 25.96(6) . . ?
O1B Ca1 C30A 150.25(6) . . ?
C30B Ca1 C30A 176.38(7) . . ?
O3A Zn1A O1A 89.58(7) . . ?
O3A Zn1A N3A 82.51(7) . . ?
O1A Zn1A N3A 172.07(7) . . ?
O3A Zn1A N1A 170.80(7) . . ?
O1A Zn1A N1A 81.93(7) . . ?
N3A Zn1A N1A 106.00(8) . . ?
O3A Zn1A N4A 96.85(8) . . ?
O1A Zn1A N4A 99.12(7) . . ?
N3A Zn1A N4A 82.50(8) . . ?
N1A Zn1A N4A 81.09(8) . . ?
O3A Zn1A N2A 103.25(7) . . ?
O1A Zn1A N2A 99.30(7) . . ?
N3A Zn1A N2A 82.03(7) . . ?
N1A Zn1A N2A 81.75(8) . . ?
N4A Zn1A N2A 152.70(7) . . ?
C30A O1A Zn1A 116.59(15) . . ?
C30A O1A Ca1 91.80(14) . . ?
Zn1A O1A Ca1 151.26(8) . . ?
C30A O2A Ca1 95.15(15) . . ?
C32A O3A Zn1A 116.88(16) . . ?
C1A N1A C8A 111.24(19) . . ?
C1A N1A C29A 111.3(2) . . ?
C8A N1A C29A 112.2(2) . . ?
C1A N1A Zn1A 107.96(15) . . ?
C8A N1A Zn1A 106.86(15) . . ?
C29A N1A Zn1A 106.99(14) . . ?
C2A N2A C3A 113.2(2) . . ?
C2A N2A C9A 109.45(19) . . ?
C3A N2A C9A 110.89(19) . . ?
C2A N2A Zn1A 105.08(14) . . ?
C3A N2A Zn1A 106.35(14) . . ?
C9A N2A Zn1A 111.68(14) . . ?
C5A N3A C4A 112.6(2) . . ?
C5A N3A C31A 111.2(2) . . ?
C4A N3A C31A 112.2(2) . . ?
C5A N3A Zn1A 107.53(15) . . ?
C4A N3A Zn1A 106.85(14) . . ?
C31A N3A Zn1A 106.05(15) . . ?
C7A N4A C6A 113.7(2) . . ?
C7A N4A C19A 110.28(19) . . ?
C6A N4A C19A 110.2(2) . . ?
C7A N4A Zn1A 108.36(15) . . ?
C6A N4A Zn1A 104.57(15) . . ?
C19A N4A Zn1A 109.41(14) . . ?
C10A N5A C18A 119.2(2) . . ?
C20A N6A C28A 119.0(2) . . ?
N1A C1A C2A 110.4(2) . . ?
N2A C2A C1A 113.3(2) . . ?
N2A C3A C4A 114.4(2) . . ?
N3A C4A C3A 111.2(2) . . ?
N3A C5A C6A 111.0(2) . . ?
N4A C6A C5A 112.5(2) . . ?
N4A C7A C8A 113.5(2) . . ?
N1A C8A C7A 111.2(2) . . ?
N2A C9A C10A 113.37(19) . . ?
N5A C10A C11A 122.1(2) . . ?
N5A C10A C9A 116.8(2) . . ?
C11A C10A C9A 121.1(2) . . ?
C12A C11A C10A 119.5(3) . . ?
C11A C12A C13A 119.9(3) . . ?
C12A C13A C18A 117.8(2) . . ?
C12A C13A C14A 123.6(3) . . ?
C18A C13A C14A 118.6(3) . . ?
C15A C14A C13A 120.9(3) . . ?
C14A C15A C16A 120.3(3) . . ?
C17A C16A C15A 120.5(3) . . ?
C16A C17A C18A 120.2(3) . . ?
N5A C18A C17A 119.0(2) . . ?
N5A C18A C13A 121.5(2) . . ?
C17A C18A C13A 119.6(2) . . ?
N4A C19A C20A 115.2(2) . . ?
N6A C20A C21A 122.4(2) . . ?
N6A C20A C19A 116.6(2) . . ?
C21A C20A C19A 121.0(2) . . ?
C22A C21A C20A 119.6(2) . . ?
C21A C22A C23A 119.4(2) . . ?
C24A C23A C22A 122.9(2) . . ?
C24A C23A C28A 119.3(2) . . ?
C22A C23A C28A 117.8(2) . . ?
C25A C24A C23A 120.2(3) . . ?
C24A C25A C26A 120.7(3) . . ?
C27A C26A C25A 120.3(3) . . ?
C26A C27A C28A 120.2(3) . . ?
N6A C28A C27A 118.8(2) . . ?
N6A C28A C23A 121.8(2) . . ?
C27A C28A C23A 119.3(2) . . ?
N1A C29A C30A 114.7(2) . . ?
O2A C30A O1A 121.8(2) . . ?
O2A C30A C29A 118.7(2) . . ?
O1A C30A C29A 119.5(2) . . ?
O2A C30A Ca1 59.66(13) . . ?
O1A C30A Ca1 62.24(12) . . ?
C29A C30A Ca1 175.20(17) . . ?
N3A C31A C32A 115.0(2) . . ?
O4A C32A O3A 125.8(3) . . ?
O4A C32A C31A 116.3(2) . . ?
O3A C32A C31A 117.8(2) . . ?
O3B Zn1B O1B 85.10(7) . . ?
O3B Zn1B N2B 108.22(8) . . ?
O1B Zn1B N2B 104.16(7) . . ?
O3B Zn1B N1B 161.36(7) . . ?
O1B Zn1B N1B 77.41(7) . . ?
N2B Zn1B N1B 82.58(8) . . ?
O3B Zn1B N4B 98.44(8) . . ?
O1B Zn1B N4B 104.44(7) . . ?
N2B Zn1B N4B 142.15(8) . . ?
N1B Zn1B N4B 80.02(8) . . ?
O3B Zn1B N3B 79.69(7) . . ?
O1B Zn1B N3B 164.72(7) . . ?
N2B Zn1B N3B 79.56(8) . . ?
N1B Zn1B N3B 117.87(7) . . ?
N4B Zn1B N3B 79.37(8) . . ?
C30B O1B Zn1B 117.89(15) . . ?
C30B O1B Ca1 89.94(14) . . ?
Zn1B O1B Ca1 152.09(8) . . ?
C30B O2B Ca1 96.33(15) . . ?
C32B O3B Zn1B 121.25(16) . . ?
C8B N1B C1B 112.71(19) . . ?
C8B N1B C29B 113.2(2) . . ?
C1B N1B C29B 109.69(19) . . ?
C8B N1B Zn1B 104.04(14) . . ?
C1B N1B Zn1B 107.28(15) . . ?
C29B N1B Zn1B 109.62(15) . . ?
C2B N2B C3B 111.12(19) . . ?
C2B N2B C9B 112.53(19) . . ?
C3B N2B C9B 111.1(2) . . ?
C2B N2B Zn1B 105.05(15) . . ?
C3B N2B Zn1B 108.14(15) . . ?
C9B N2B Zn1B 108.64(14) . . ?
C4B N3B C5B 113.00(19) . . ?
C4B N3B C31B 111.0(2) . . ?
C5B N3B C31B 112.3(2) . . ?
C4B N3B Zn1B 107.66(15) . . ?
C5B N3B Zn1B 106.28(15) . . ?
C31B N3B Zn1B 106.10(14) . . ?
C6B N4B C7B 112.4(2) . . ?
C6B N4B C19B 111.17(19) . . ?
C7B N4B C19B 112.5(2) . . ?
C6B N4B Zn1B 107.50(15) . . ?
C7B N4B Zn1B 108.71(15) . . ?
C19B N4B Zn1B 104.03(14) . . ?
C10B N5B C18B 118.6(2) . . ?
C20B N6B C28B 118.3(2) . . ?
N1B C1B C2B 111.8(2) . . ?
N2B C2B C1B 111.4(2) . . ?
N2B C3B C4B 111.1(2) . . ?
N3B C4B C3B 110.0(2) . . ?
N3B C5B C6B 109.6(2) . . ?
N4B C6B C5B 111.2(2) . . ?
N4B C7B C8B 113.4(2) . . ?
N1B C8B C7B 111.3(2) . . ?
N2B C9B C10B 114.6(2) . . ?
N5B C10B C11B 122.8(2) . . ?
N5B C10B C9B 116.0(2) . . ?
C11B C10B C9B 121.2(2) . . ?
C12B C11B C10B 119.2(3) . . ?
C11B C12B C13B 119.8(3) . . ?
C12B C13B C18B 117.5(2) . . ?
C12B C13B C14B 124.1(3) . . ?
C18B C13B C14B 118.3(3) . . ?
C15B C14B C13B 120.6(3) . . ?
C14B C15B C16B 121.4(3) . . ?
C17B C16B C15B 120.0(3) . . ?
C16B C17B C18B 120.1(3) . . ?
N5B C18B C17B 118.3(3) . . ?
N5B C18B C13B 122.1(2) . . ?
C17B C18B C13B 119.6(3) . . ?
N4B C19B C20B 115.7(2) . . ?
N6B C20B C21B 123.1(2) . . ?
N6B C20B C19B 115.6(2) . . ?
C21B C20B C19B 121.3(2) . . ?
C22B C21B C20B 119.3(3) . . ?
C21B C22B C23B 119.8(3) . . ?
C22B C23B C24B 123.8(3) . . ?
C22B C23B C28B 117.7(3) . . ?
C24B C23B C28B 118.5(3) . . ?
C25B C24B C23B 120.9(4) . . ?
C24B C25B C26B 120.4(3) . . ?
C27B C26B C25B 120.9(3) . . ?
C26B C27B C28B 119.4(4) . . ?
N6B C28B C27B 118.4(3) . . ?
N6B C28B C23B 121.8(3) . . ?
C27B C28B C23B 119.8(3) . . ?
N1B C29B C30B 109.8(2) . . ?
O2B C30B O1B 122.3(2) . . ?
O2B C30B C29B 119.7(2) . . ?
O1B C30B C29B 118.0(2) . . ?
O2B C30B Ca1 58.42(13) . . ?
O1B C30B Ca1 63.92(12) . . ?
C29B C30B Ca1 174.33(17) . . ?
N3B C31B C32B 115.2(2) . . ?
O4B C32B O3B 125.1(2) . . ?
O4B C32B C31B 117.3(2) . . ?
O3B C32B C31B 117.5(2) . . ?
O10 Cl1 O11 110.28(19) . . ?
O10 Cl1 O12 108.94(16) . . ?
O11 Cl1 O12 110.22(17) . . ?
O10 Cl1 O13 108.5(2) . . ?
O11 Cl1 O13 109.19(18) . . ?
O12 Cl1 O13 109.72(19) . . ?
O24B Cl2 O23B 127.0(6) . . ?
O24A Cl2 O23A 119.3(4) . . ?
O24A Cl2 O21A 113.4(4) . . ?
O23A Cl2 O21A 106.6(4) . . ?
O24A Cl2 O22A 111.3(3) . . ?
O23A Cl2 O22A 101.7(3) . . ?
O21A Cl2 O22A 102.8(3) . . ?
O24B Cl2 O22B 105.9(6) . . ?
O23B Cl2 O22B 111.4(5) . . ?
O24B Cl2 O21B 106.8(6) . . ?
O23B Cl2 O21B 110.0(4) . . ?
O22B Cl2 O21B 89.1(4) . . ?

_refine_diff_density_max         1.084
_refine_diff_density_min         -1.624
_refine_diff_density_rms         0.092



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_ZnL4-ClO4-H2O
_database_code_depnum_ccdc_archive 'CCDC 2375276'
loop_
_audit_author_name
_audit_author_address
'Patrizia Rossi'
;University of Firenze
Italy
;
_audit_update_record             
;
2024-10-17 deposited with the CCDC.	2024-12-11 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT029_ZnL4-ClO4-H2O       
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.937 Why?
RESPONSE: the quality of the crystals was not very good.
The data reported are the best set we were able to obtain
;
_vrf_PLAT910_ZnL4-ClO4-H2O       
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min). 26 Note
RESPONSE: this is probably due to the beamstop mask
;
_vrf_PLAT911_ZnL4-ClO4-H2O       
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L= 0.600 414 Report
RESPONSE: this is probably due to the beamstop mask
;
# end Validation Reply Form

_publ_section_title_             
;
Zn(II)/Cd(II) selective binding and fluorescence sensing 
by using macrocyclic tetra-amines with different fluorophores. 
Clues for design of selective chemosensors for transition metals.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H36 Cl2 N6 O11 Zn'
_chemical_formula_weight         768.90

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   10.4810(7)
_cell_length_b                   16.9390(10)
_cell_length_c                   17.6970(10)
_cell_angle_alpha                90
_cell_angle_beta                 94.523(6)
_cell_angle_gamma                90
_cell_volume                     3132.1(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    2938
_cell_measurement_theta_min      4.1495
_cell_measurement_theta_max      26.7422

_exptl_crystal_description       prism
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.631
_exptl_crystal_F_000             1592
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_exptl_absorpt_coefficient_mu    1.026
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.81560
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15292
_diffrn_reflns_av_unetI/netI     0.1198
_diffrn_reflns_av_R_equivalents  0.0772
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         4.158
_diffrn_reflns_theta_max         26.801
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.808
_diffrn_measured_fraction_theta_full 0.937
_diffrn_reflns_Laue_measured_fraction_max 0.808
_diffrn_reflns_Laue_measured_fraction_full 0.937
_diffrn_reflns_point_group_measured_fraction_max 0.808
_diffrn_reflns_point_group_measured_fraction_full 0.937
_reflns_number_total             5414
_reflns_number_gt                3371
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_cell_refinement       
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_data_reduction        
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_structure_solution    'SIR2004 (Burla, 2005)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Mercury 3.10.1'
_computing_publication_material  'PARST(Nardelli, 1995)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0837P)²+27.0496P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5414
_refine_ls_number_parameters     446
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.1520
_refine_ls_R_factor_gt           0.0995
_refine_ls_wR_factor_ref         0.2647
_refine_ls_wR_factor_gt          0.2377
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_restrained_S_all      1.109
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
O1 O 0.3653(6) 0.2016(4) 0.2493(4) 0.0372(17) Uani 1 1 d . . . . .
H1 H 0.436910 0.194222 0.273025 0.056 Uiso 1 1 calc R U . . .
O2 O 0.0586(6) 0.0955(4) 0.0508(4) 0.0358(17) Uani 1 1 d . . . . .
H2 H 0.002369 0.104040 0.015189 0.054 Uiso 1 1 calc R U . . .
Zn1 Zn 0.11993(11) 0.11977(7) 0.21843(6) 0.0318(4) Uani 1 1 d . . . . .
N2 N -0.0682(8) 0.1834(5) 0.2143(4) 0.036(2) Uani 1 1 d . . . . .
N3 N 0.1354(8) 0.1743(5) 0.3296(4) 0.038(2) Uani 1 1 d . . . . .
H3N H 0.182546 0.225137 0.324605 0.046 Uiso 1 1 calc R U . . .
N4 N 0.2067(8) 0.0214(5) 0.2891(4) 0.0308(19) Uani 1 1 d . . . . .
N1 N -0.0127(7) 0.0252(5) 0.1846(4) 0.0297(19) Uani 1 1 d . . . . .
H1N H 0.016721 0.001998 0.136990 0.036 Uiso 1 1 calc R U . . .
N5 N 0.1519(8) 0.2344(5) 0.1593(4) 0.0310(19) Uani 1 1 d . . . . .
N6 N 0.2666(8) 0.0655(5) 0.1501(4) 0.033(2) Uani 1 1 d . . . . .
C1 C 0.2124(11) 0.1260(6) 0.3861(5) 0.041(3) Uani 1 1 d . . . . .
H1A H 0.187665 0.138465 0.437611 0.050 Uiso 1 1 calc R U . . .
H1B H 0.304278 0.138776 0.384194 0.050 Uiso 1 1 calc R U . . .
C2 C 0.1911(10) 0.0380(6) 0.3700(5) 0.039(3) Uani 1 1 d . . . . .
H2A H 0.253537 0.006531 0.402242 0.046 Uiso 1 1 calc R U . . .
H2B H 0.103939 0.022775 0.382263 0.046 Uiso 1 1 calc R U . . .
C3 C 0.1405(9) -0.0517(6) 0.2628(6) 0.035(2) Uani 1 1 d . . . . .
H3A H 0.150623 -0.092203 0.303159 0.042 Uiso 1 1 calc R U . . .
H3B H 0.180050 -0.072292 0.217766 0.042 Uiso 1 1 calc R U . . .
C4 C 0.0003(9) -0.0371(6) 0.2427(5) 0.033(2) Uani 1 1 d . . . . .
H4A H -0.041548 -0.086140 0.223086 0.040 Uiso 1 1 calc R U . . .
H4B H -0.041479 -0.020314 0.288362 0.040 Uiso 1 1 calc R U . . .
C5 C -0.1450(9) 0.0540(6) 0.1661(6) 0.037(2) Uani 1 1 d . . . . .
H5A H -0.156641 0.070306 0.112292 0.044 Uiso 1 1 calc R U . . .
H5B H -0.207403 0.011678 0.174717 0.044 Uiso 1 1 calc R U . . .
C6 C -0.1650(10) 0.1217(6) 0.2159(5) 0.033(2) Uani 1 1 d . . . . .
H6A H -0.249792 0.145154 0.200932 0.039 Uiso 1 1 calc R U . . .
H6B H -0.166704 0.102376 0.268579 0.039 Uiso 1 1 calc R U . . .
C7 C -0.0646(11) 0.2340(6) 0.2831(6) 0.042(3) Uani 1 1 d . . . . .
H7A H -0.153170 0.245006 0.295880 0.051 Uiso 1 1 calc R U . . .
H7B H -0.023538 0.285055 0.272487 0.051 Uiso 1 1 calc R U . . .
C8 C 0.0090(11) 0.1944(6) 0.3500(6) 0.042(3) Uani 1 1 d . . . . .
H8A H 0.015125 0.230473 0.394132 0.050 Uiso 1 1 calc R U . . .
H8B H -0.036507 0.146011 0.364228 0.050 Uiso 1 1 calc R U . . .
C9 C -0.0819(9) 0.2315(6) 0.1462(5) 0.033(2) Uani 1 1 d . . . . .
H9A H -0.138095 0.276998 0.154840 0.040 Uiso 1 1 calc R U . . .
H9B H -0.123161 0.199774 0.104109 0.040 Uiso 1 1 calc R U . . .
C10 C 0.3428(9) 0.0177(6) 0.2737(5) 0.035(2) Uani 1 1 d . . . . .
H10A H 0.375116 -0.036508 0.283543 0.043 Uiso 1 1 calc R U . . .
H10B H 0.392595 0.053835 0.308765 0.043 Uiso 1 1 calc R U . . .
C11 C 0.0482(10) 0.2618(6) 0.1237(6) 0.035(2) Uani 1 1 d . . . . .
C12 C 0.0457(10) 0.3165(6) 0.0627(5) 0.034(2) Uani 1 1 d . . . . .
H12 H -0.032677 0.336301 0.039482 0.041 Uiso 1 1 calc R U . . .
C13 C 0.1590(12) 0.3391(6) 0.0393(6) 0.044(3) Uani 1 1 d . . . . .
H13 H 0.160082 0.373578 -0.002947 0.053 Uiso 1 1 calc R U . . .
C14 C 0.2781(10) 0.3130(6) 0.0759(5) 0.033(2) Uani 1 1 d . . . . .
C15 C 0.2691(10) 0.2626(5) 0.1400(5) 0.031(2) Uani 1 1 d . . . . .
C16 C 0.3993(12) 0.3383(6) 0.0564(6) 0.043(3) Uani 1 1 d . . . . .
H16 H 0.405830 0.371840 0.013899 0.052 Uiso 1 1 calc R U . . .
C17 C 0.5061(12) 0.3150(6) 0.0979(7) 0.048(3) Uani 1 1 d . . . . .
H17 H 0.587861 0.329578 0.082869 0.057 Uiso 1 1 calc R U . . .
C18 C 0.4961(10) 0.2687(6) 0.1639(6) 0.041(3) Uani 1 1 d . . . . .
H18 H 0.571683 0.254924 0.194113 0.049 Uiso 1 1 calc R U . . .
C19 C 0.3810(10) 0.2436(6) 0.1849(6) 0.033(2) Uani 1 1 d . . . . .
C20 C 0.3636(9) 0.0401(6) 0.1938(5) 0.033(2) Uani 1 1 d . . . . .
C21 C 0.4909(10) 0.0365(6) 0.1692(6) 0.039(3) Uani 1 1 d . . . . .
H21 H 0.559385 0.016362 0.202036 0.046 Uiso 1 1 calc R U . . .
C22 C 0.5118(11) 0.0617(6) 0.0997(6) 0.044(3) Uani 1 1 d . . . . .
H22 H 0.596607 0.062971 0.084319 0.052 Uiso 1 1 calc R U . . .
C23 C 0.4082(10) 0.0866(6) 0.0487(5) 0.034(2) Uani 1 1 d . . . . .
C24 C 0.2854(9) 0.0854(5) 0.0751(5) 0.028(2) Uani 1 1 d . . . . .
C25 C 0.1779(10) 0.1028(5) 0.0244(5) 0.035(2) Uani 1 1 d . . . . .
C26 C 0.1941(11) 0.1214(6) -0.0496(6) 0.039(3) Uani 1 1 d . . . . .
H26 H 0.121780 0.130448 -0.084277 0.047 Uiso 1 1 calc R U . . .
C27 C 0.3173(12) 0.1271(7) -0.0736(6) 0.047(3) Uani 1 1 d . . . . .
H27 H 0.327851 0.144450 -0.123804 0.057 Uiso 1 1 calc R U . . .
C28 C 0.4240(11) 0.1082(6) -0.0268(6) 0.043(3) Uani 1 1 d . . . . .
H28 H 0.506809 0.109740 -0.045016 0.051 Uiso 1 1 calc R U . . .
O1W O -0.4155(8) 0.1972(5) 0.3419(4) 0.052(2) Uani 1 1 d D . . . .
H1WA H -0.409(12) 0.153(2) 0.363(5) 0.063 Uiso 1 1 d D U . . .
H1WB H -0.427(12) 0.230(4) 0.376(4) 0.063 Uiso 1 1 d D U . . .
Cl1 Cl -0.2888(2) -0.01614(16) 0.38411(14) 0.0387(7) Uani 1 1 d . . . . .
O11 O -0.3934(10) 0.0350(6) 0.3861(6) 0.096(4) Uani 1 1 d . . . . .
O12 O -0.2956(8) -0.0581(5) 0.3154(5) 0.062(2) Uani 1 1 d . . . . .
O13 O -0.1711(9) 0.0265(6) 0.3958(5) 0.072(3) Uani 1 1 d . . . . .
O14 O -0.2920(9) -0.0709(6) 0.4430(5) 0.082(3) Uani 1 1 d . . . . .
Cl2 Cl -0.2073(2) 0.15617(15) -0.07036(13) 0.0350(6) Uani 1 1 d . . . . .
O21 O -0.3032(7) 0.1482(4) -0.1320(4) 0.0430(18) Uiso 1 1 d . . . . .
O22A O -0.2694(16) 0.1635(18) -0.0006(9) 0.040(6) Uiso 0.51(4) 1 d . . P A 1
O23A O -0.126(2) 0.0823(13) -0.0658(13) 0.029(5) Uiso 0.51(4) 1 d . . P A 1
O24A O -0.1200(16) 0.2186(10) -0.0775(15) 0.028(5) Uiso 0.51(4) 1 d . . P A 1
O22B O -0.250(6) 0.111(5) -0.007(3) 0.05(2) Uiso 0.12(2) 1 d . . P A 2
O23B O -0.161(6) 0.229(3) -0.044(4) 0.028(17) Uiso 0.12(2) 1 d . . P A 2
O24B O -0.098(8) 0.110(6) -0.079(5) 0.06(3) Uiso 0.12(2) 1 d . . P A 2
O22C O -0.110(2) 0.2047(16) -0.106(2) 0.049(8) Uiso 0.38(4) 1 d . . P A 3
O23C O -0.258(2) 0.199(2) -0.0112(13) 0.046(8) Uiso 0.38(4) 1 d . . P A 3
O24C O -0.158(3) 0.0846(14) -0.0491(15) 0.029(7) Uiso 0.38(4) 1 d . . P A 3


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
O1 C19 1.365(12) . ?
O2 C25 1.375(12) . ?
Zn1 N3 2.168(8) . ?
Zn1 N1 2.174(8) . ?
Zn1 N6 2.228(8) . ?
Zn1 N4 2.234(8) . ?
Zn1 N2 2.243(8) . ?
Zn1 N5 2.243(8) . ?
N2 C9 1.452(12) . ?
N2 C6 1.458(12) . ?
N2 C7 1.486(13) . ?
N3 C8 1.442(13) . ?
N3 C1 1.481(13) . ?
N4 C10 1.475(12) . ?
N4 C3 1.477(12) . ?
N4 C2 1.481(12) . ?
N1 C4 1.473(12) . ?
N1 C5 1.482(12) . ?
N5 C11 1.298(12) . ?
N5 C15 1.386(13) . ?
N6 C20 1.301(12) . ?
N6 C24 1.398(11) . ?
C1 C2 1.530(14) . ?
C3 C4 1.504(13) . ?
C5 C6 1.472(13) . ?
C7 C8 1.519(14) . ?
C9 C11 1.539(14) . ?
C10 C20 1.497(13) . ?
C11 C12 1.421(14) . ?
C12 C13 1.344(15) . ?
C13 C14 1.430(15) . ?
C14 C16 1.409(15) . ?
C14 C15 1.428(13) . ?
C15 C19 1.401(13) . ?
C16 C17 1.347(16) . ?
C17 C18 1.417(15) . ?
C18 C19 1.359(14) . ?
C20 C21 1.437(14) . ?
C21 C22 1.337(14) . ?
C22 C23 1.420(14) . ?
C23 C24 1.404(13) . ?
C23 C28 1.408(14) . ?
C24 C25 1.414(13) . ?
C25 C26 1.370(14) . ?
C26 C27 1.394(15) . ?
C27 C28 1.377(15) . ?
Cl1 O14 1.397(9) . ?
Cl1 O11 1.399(10) . ?
Cl1 O12 1.405(8) . ?
Cl1 O13 1.431(8) . ?
Cl2 O24C 1.36(2) . ?
Cl2 O23B 1.40(5) . ?
Cl2 O24B 1.40(8) . ?
Cl2 O24A 1.410(15) . ?
Cl2 O23C 1.41(2) . ?
Cl2 O21 1.430(7) . ?
Cl2 O22A 1.446(17) . ?
Cl2 O22B 1.45(6) . ?
Cl2 O22C 1.49(3) . ?
Cl2 O23A 1.51(2) . ?

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
N3 Zn1 N1 124.4(3) . . ?
N3 Zn1 N6 131.5(3) . . ?
N1 Zn1 N6 90.0(3) . . ?
N3 Zn1 N4 79.2(3) . . ?
N1 Zn1 N4 80.1(3) . . ?
N6 Zn1 N4 74.2(3) . . ?
N3 Zn1 N2 80.1(3) . . ?
N1 Zn1 N2 78.7(3) . . ?
N6 Zn1 N2 145.4(3) . . ?
N4 Zn1 N2 134.0(3) . . ?
N3 Zn1 N5 92.9(3) . . ?
N1 Zn1 N5 128.7(3) . . ?
N6 Zn1 N5 88.2(3) . . ?
N4 Zn1 N5 146.9(3) . . ?
N2 Zn1 N5 74.5(3) . . ?
C9 N2 C6 113.2(8) . . ?
C9 N2 C7 110.5(8) . . ?
C6 N2 C7 111.8(8) . . ?
C9 N2 Zn1 109.0(6) . . ?
C6 N2 Zn1 105.4(6) . . ?
C7 N2 Zn1 106.6(6) . . ?
C8 N3 C1 115.1(8) . . ?
C8 N3 Zn1 108.9(6) . . ?
C1 N3 Zn1 112.0(6) . . ?
C10 N4 C3 110.2(8) . . ?
C10 N4 C2 111.6(8) . . ?
C3 N4 C2 112.3(7) . . ?
C10 N4 Zn1 106.5(5) . . ?
C3 N4 Zn1 106.8(6) . . ?
C2 N4 Zn1 109.1(6) . . ?
C4 N1 C5 115.0(8) . . ?
C4 N1 Zn1 108.3(6) . . ?
C5 N1 Zn1 112.7(6) . . ?
C11 N5 C15 118.8(8) . . ?
C11 N5 Zn1 112.7(7) . . ?
C15 N5 Zn1 125.5(6) . . ?
C20 N6 C24 118.8(8) . . ?
C20 N6 Zn1 110.8(6) . . ?
C24 N6 Zn1 124.8(6) . . ?
N3 C1 C2 110.4(8) . . ?
N4 C2 C1 109.9(8) . . ?
N4 C3 C4 111.2(8) . . ?
N1 C4 C3 108.5(8) . . ?
C6 C5 N1 107.4(8) . . ?
N2 C6 C5 114.6(8) . . ?
N2 C7 C8 111.2(8) . . ?
N3 C8 C7 109.2(8) . . ?
N2 C9 C11 111.8(8) . . ?
N4 C10 C20 112.3(8) . . ?
N5 C11 C12 124.5(10) . . ?
N5 C11 C9 118.6(9) . . ?
C12 C11 C9 116.8(9) . . ?
C13 C12 C11 117.1(10) . . ?
C12 C13 C14 122.3(10) . . ?
C16 C14 C15 119.5(10) . . ?
C16 C14 C13 124.5(10) . . ?
C15 C14 C13 115.8(10) . . ?
N5 C15 C19 120.0(8) . . ?
N5 C15 C14 121.1(9) . . ?
C19 C15 C14 118.9(10) . . ?
C17 C16 C14 120.3(10) . . ?
C16 C17 C18 119.9(11) . . ?
C19 C18 C17 121.6(10) . . ?
C18 C19 O1 124.1(9) . . ?
C18 C19 C15 119.6(10) . . ?
O1 C19 C15 116.3(9) . . ?
N6 C20 C21 122.4(9) . . ?
N6 C20 C10 118.7(9) . . ?
C21 C20 C10 118.8(9) . . ?
C22 C21 C20 119.2(10) . . ?
C21 C22 C23 120.4(10) . . ?
C24 C23 C28 119.9(10) . . ?
C24 C23 C22 117.4(9) . . ?
C28 C23 C22 122.6(10) . . ?
N6 C24 C23 121.3(9) . . ?
N6 C24 C25 119.2(9) . . ?
C23 C24 C25 119.5(9) . . ?
C26 C25 O2 122.0(9) . . ?
C26 C25 C24 120.1(10) . . ?
O2 C25 C24 117.8(8) . . ?
C25 C26 C27 119.7(10) . . ?
C28 C27 C26 121.8(10) . . ?
C27 C28 C23 118.8(10) . . ?
O14 Cl1 O11 109.1(7) . . ?
O14 Cl1 O12 107.8(6) . . ?
O11 Cl1 O12 110.4(6) . . ?
O14 Cl1 O13 107.4(6) . . ?
O11 Cl1 O13 110.7(6) . . ?
O12 Cl1 O13 111.3(5) . . ?
O23B Cl2 O24B 105(4) . . ?
O24C Cl2 O23C 114.2(14) . . ?
O24C Cl2 O21 110.7(9) . . ?
O23B Cl2 O21 123(2) . . ?
O24B Cl2 O21 113(3) . . ?
O24A Cl2 O21 115.1(8) . . ?
O23C Cl2 O21 109.3(9) . . ?
O24A Cl2 O22A 110.5(11) . . ?
O21 Cl2 O22A 108.9(7) . . ?
O23B Cl2 O22B 110(4) . . ?
O24B Cl2 O22B 96(4) . . ?
O21 Cl2 O22B 107(2) . . ?
O24C Cl2 O22C 110.8(14) . . ?
O23C Cl2 O22C 110.0(14) . . ?
O21 Cl2 O22C 101.2(13) . . ?
O24A Cl2 O23A 105.0(11) . . ?
O21 Cl2 O23A 108.7(7) . . ?
O22A Cl2 O23A 108.3(11) . . ?

_refine_diff_density_max         1.287
_refine_diff_density_min         -0.665
_refine_diff_density_rms         0.132



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_PbL4-ClO4-2H2O
_database_code_depnum_ccdc_archive 'CCDC 2375277'
loop_
_audit_author_name
_audit_author_address
'Patrizia Rossi'
;University of Firenze
Italy
;
_audit_update_record             
;
2024-08-02 deposited with the CCDC.	2024-12-11 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT910_PbL4-ClO4-2H2O      
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min). 23 Note
RESPONSE: this is probably due to the beamstop mask
;
# end Validation Reply Form

_publ_section_title_             
;
Zn(II)/Cd(II) selective binding and fluorescence sensing 
by using macrocyclic tetra-amines with different fluorophores. 
Clues for design of selective chemosensors for transition metals.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H35 Cl N6 O7 Pb'
_chemical_formula_weight         810.26

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'
Pb Pb -3.3944 10.1111 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   12.1623(4)
_cell_length_b                   16.0748(5)
_cell_length_c                   15.0537(5)
_cell_angle_alpha                90
_cell_angle_beta                 100.065(3)
_cell_angle_gamma                90
_cell_volume                     2897.80(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    6158
_cell_measurement_theta_min      4.1582
_cell_measurement_theta_max      29.3060

_exptl_crystal_description       prism
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.857
_exptl_crystal_F_000             1600
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.19
_exptl_absorpt_coefficient_mu    5.972
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.56060
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            20089
_diffrn_reflns_av_unetI/netI     0.0644
_diffrn_reflns_av_R_equivalents  0.0516
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         4.167
_diffrn_reflns_theta_max         29.371
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.854
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.854
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.854
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             6818
_reflns_number_gt                5412
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_cell_refinement       
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_data_reduction        
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_structure_solution    'SIR25004 (Burla, 2005)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Mercury 3.10.1'
_computing_publication_material  'PARST(Nardelli, 1995)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0246P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6818
_refine_ls_number_parameters     409
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0355
_refine_ls_wR_factor_ref         0.0744
_refine_ls_wR_factor_gt          0.0671
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
Cl1 Cl 0.40780(11) 0.28877(9) 0.41337(9) 0.0394(3) Uani 1 1 d . . . . .
O1A O 0.4033(14) 0.2946(9) 0.3189(10) 0.030(4) Uiso 0.33 1 d . . P A 1
O2A O 0.517(2) 0.305(2) 0.4646(19) 0.032(7) Uiso 0.33 1 d . . P A 1
O3A O 0.3198(10) 0.3383(8) 0.4394(9) 0.036(3) Uiso 0.33 1 d . . P A 1
O4A O 0.3881(13) 0.2020(10) 0.4238(12) 0.042(4) Uiso 0.33 1 d . . P A 1
O1B O 0.3464(8) 0.3733(6) 0.4230(8) 0.031(2) Uiso 0.34 1 d . . P A 2
O2B O 0.3521(10) 0.2245(8) 0.4366(9) 0.039(3) Uiso 0.34 1 d . . P A 2
O3B O 0.4439(10) 0.2987(9) 0.3244(9) 0.037(4) Uiso 0.34 1 d . . P A 2
O4B O 0.5033(12) 0.2949(14) 0.4772(11) 0.023(4) Uiso 0.34 1 d . . P A 2
O1C O 0.4065(12) 0.1894(9) 0.3941(11) 0.051(4) Uiso 0.33 1 d . . P A 3
O2C O 0.3091(10) 0.2911(9) 0.4528(9) 0.051(3) Uiso 0.33 1 d . . P A 3
O3C O 0.5156(19) 0.3202(13) 0.4690(17) 0.029(5) Uiso 0.33 1 d . . P A 3
O4C O 0.3970(12) 0.3226(8) 0.3256(10) 0.033(3) Uiso 0.33 1 d . . P A 3
O1WA O 0.7074(8) 0.3415(8) 0.3469(18) 0.041(3) Uiso 0.55(6) 1 d . . P B 1
O1WB O 0.7163(9) 0.3520(8) 0.3767(19) 0.033(4) Uiso 0.45(6) 1 d . . P B 2
Pb1 Pb 0.02685(2) 0.17268(2) 0.35267(2) 0.01864(6) Uani 1 1 d . . . . .
N1 N 0.1872(3) 0.1845(2) 0.2435(3) 0.0247(9) Uani 1 1 d D . . . .
H1N H 0.234(3) 0.192(3) 0.295(2) 0.030 Uiso 1 1 d D U . . .
N2 N 0.0149(3) 0.3109(2) 0.2448(3) 0.0190(8) Uani 1 1 d . . . . .
N3 N -0.1047(3) 0.1526(2) 0.2165(3) 0.0198(8) Uani 1 1 d D . . . .
H3N H -0.156(3) 0.126(2) 0.237(3) 0.024 Uiso 1 1 d D U . . .
N4 N 0.0735(3) 0.0289(2) 0.2726(3) 0.0225(9) Uani 1 1 d . . . . .
N5 N -0.0013(3) 0.3520(2) 0.4461(3) 0.0227(9) Uani 1 1 d . . . . .
N6 N -0.0777(3) 0.0410(2) 0.3865(2) 0.0183(8) Uani 1 1 d . . . . .
O1 O -0.0826(3) 0.2634(2) 0.5746(2) 0.0303(8) Uani 1 1 d D . . . .
H1O H -0.085(4) 0.253(3) 0.5202(15) 0.036 Uiso 1 1 d D U . . .
O2 O -0.1531(2) 0.19787(18) 0.4052(2) 0.0245(7) Uani 1 1 d . . . . .
C1 C 0.1830(4) 0.2580(3) 0.1866(3) 0.0270(11) Uani 1 1 d . . . . .
H1A H 0.140289 0.245349 0.125896 0.032 Uiso 1 1 calc R U . . .
H1B H 0.259739 0.274021 0.179804 0.032 Uiso 1 1 calc R U . . .
C2 C 0.1282(3) 0.3296(3) 0.2276(3) 0.0208(10) Uani 1 1 d . . . . .
H2A H 0.175903 0.345592 0.285237 0.025 Uiso 1 1 calc R U . . .
H2B H 0.123884 0.378061 0.186472 0.025 Uiso 1 1 calc R U . . .
C3 C -0.0640(4) 0.2918(3) 0.1606(3) 0.0244(10) Uani 1 1 d . . . . .
H3A H -0.022690 0.266735 0.116135 0.029 Uiso 1 1 calc R U . . .
H3B H -0.099121 0.343867 0.134546 0.029 Uiso 1 1 calc R U . . .
C4 C -0.1542(3) 0.2318(2) 0.1792(3) 0.0235(11) Uani 1 1 d . . . . .
H4A H -0.196631 0.257379 0.222571 0.028 Uiso 1 1 calc R U . . .
H4B H -0.206835 0.220727 0.122480 0.028 Uiso 1 1 calc R U . . .
C5 C -0.0606(4) 0.1009(3) 0.1500(3) 0.0254(11) Uani 1 1 d . . . . .
H5A H -0.001820 0.132211 0.126466 0.030 Uiso 1 1 calc R U . . .
H5B H -0.121440 0.088986 0.098759 0.030 Uiso 1 1 calc R U . . .
C6 C -0.0124(4) 0.0195(3) 0.1899(3) 0.0245(10) Uani 1 1 d . . . . .
H6A H -0.073984 -0.015303 0.204405 0.029 Uiso 1 1 calc R U . . .
H6B H 0.021300 -0.010333 0.143740 0.029 Uiso 1 1 calc R U . . .
C7 C 0.1881(4) 0.0313(3) 0.2526(4) 0.0296(12) Uani 1 1 d . . . . .
H7A H 0.200736 -0.019432 0.218514 0.036 Uiso 1 1 calc R U . . .
H7B H 0.241662 0.030261 0.310274 0.036 Uiso 1 1 calc R U . . .
C8 C 0.2129(4) 0.1074(3) 0.1985(4) 0.0318(12) Uani 1 1 d . . . . .
H8A H 0.292619 0.107238 0.192475 0.038 Uiso 1 1 calc R U . . .
H8B H 0.167425 0.104884 0.137233 0.038 Uiso 1 1 calc R U . . .
C9 C -0.0277(4) 0.3835(2) 0.2875(3) 0.0227(10) Uani 1 1 d . . . . .
H9A H -0.108610 0.375622 0.286802 0.027 Uiso 1 1 calc R U . . .
H9B H -0.018878 0.433416 0.250913 0.027 Uiso 1 1 calc R U . . .
C10 C 0.0289(3) 0.3993(3) 0.3833(3) 0.0215(10) Uani 1 1 d . . . . .
C11 C 0.1081(3) 0.4637(3) 0.4047(4) 0.0266(11) Uani 1 1 d . . . . .
H11 H 0.130132 0.495785 0.357762 0.032 Uiso 1 1 calc R U . . .
C12 C 0.1526(4) 0.4798(3) 0.4917(4) 0.0291(12) Uani 1 1 d . . . . .
H12 H 0.205947 0.523155 0.505889 0.035 Uiso 1 1 calc R U . . .
C13 C 0.1200(3) 0.4325(3) 0.5611(4) 0.0252(11) Uani 1 1 d . . . . .
C14 C 0.1552(4) 0.4474(3) 0.6533(4) 0.0303(12) Uani 1 1 d . . . . .
H14 H 0.208919 0.489444 0.672708 0.036 Uiso 1 1 calc R U . . .
C15 C 0.1121(4) 0.4013(3) 0.7155(4) 0.0347(13) Uani 1 1 d . . . . .
H15 H 0.135611 0.412558 0.777895 0.042 Uiso 1 1 calc R U . . .
C16 C 0.0340(4) 0.3377(3) 0.6893(4) 0.0289(12) Uani 1 1 d . . . . .
H16 H 0.006365 0.305660 0.733672 0.035 Uiso 1 1 calc R U . . .
C17 C -0.0023(4) 0.3219(3) 0.5994(4) 0.0250(11) Uani 1 1 d . . . . .
C18 C 0.0411(4) 0.3682(3) 0.5332(3) 0.0238(10) Uani 1 1 d . . . . .
C19 C 0.0657(4) -0.0411(3) 0.3333(3) 0.0252(11) Uani 1 1 d . . . . .
H19A H 0.132176 -0.041640 0.381801 0.030 Uiso 1 1 calc R U . . .
H19B H 0.064545 -0.093953 0.299342 0.030 Uiso 1 1 calc R U . . .
C20 C -0.0389(4) -0.0348(3) 0.3747(3) 0.0232(10) Uani 1 1 d . . . . .
C21 C -0.0916(4) -0.1062(3) 0.4023(3) 0.0289(12) Uani 1 1 d . . . . .
H21 H -0.062073 -0.159922 0.394681 0.035 Uiso 1 1 calc R U . . .
C22 C -0.1845(4) -0.0976(3) 0.4398(3) 0.0284(12) Uani 1 1 d . . . . .
H22 H -0.219689 -0.145689 0.458534 0.034 Uiso 1 1 calc R U . . .
C23 C -0.2297(4) -0.0183(3) 0.4514(3) 0.0239(10) Uani 1 1 d . . . . .
C24 C -0.3267(4) -0.0038(3) 0.4877(3) 0.0283(11) Uani 1 1 d . . . . .
H24 H -0.366080 -0.049126 0.507804 0.034 Uiso 1 1 calc R U . . .
C25 C -0.3641(4) 0.0758(3) 0.4939(3) 0.0288(11) Uani 1 1 d . . . . .
H25 H -0.430903 0.084985 0.517122 0.035 Uiso 1 1 calc R U . . .
C26 C -0.3065(4) 0.1440(3) 0.4670(3) 0.0253(10) Uani 1 1 d . . . . .
H26 H -0.334582 0.198470 0.472952 0.030 Uiso 1 1 calc R U . . .
C27 C -0.2092(3) 0.1338(3) 0.4316(3) 0.0217(10) Uani 1 1 d . . . . .
C28 C -0.1713(3) 0.0511(3) 0.4230(3) 0.0191(10) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Cl1 O2B 1.316(12) . ?
Cl1 O4B 1.376(15) . ?
Cl1 O4C 1.414(14) . ?
Cl1 O1A 1.416(15) . ?
Cl1 O4A 1.428(15) . ?
Cl1 O2C 1.430(13) . ?
Cl1 O3A 1.441(12) . ?
Cl1 O2A 1.44(3) . ?
Cl1 O3B 1.489(14) . ?
Cl1 O3C 1.51(2) . ?
Cl1 O1B 1.569(10) . ?
Cl1 O1C 1.623(14) . ?
Pb1 N3 2.391(4) . ?
Pb1 O2 2.487(3) . ?
Pb1 N6 2.566(3) . ?
Pb1 N4 2.712(4) . ?
Pb1 N2 2.741(3) . ?
Pb1 N1 2.767(4) . ?
N1 C1 1.455(6) . ?
N1 C8 1.473(6) . ?
N2 C9 1.470(5) . ?
N2 C2 1.477(5) . ?
N2 C3 1.481(5) . ?
N3 C5 1.472(6) . ?
N3 C4 1.476(5) . ?
N4 C19 1.464(6) . ?
N4 C7 1.478(6) . ?
N4 C6 1.486(5) . ?
N5 C10 1.315(6) . ?
N5 C18 1.348(6) . ?
N6 C20 1.329(5) . ?
N6 C28 1.357(6) . ?
O1 C17 1.360(5) . ?
O2 C27 1.333(5) . ?
C1 C2 1.515(6) . ?
C3 C4 1.523(6) . ?
C5 C6 1.513(6) . ?
C7 C8 1.528(7) . ?
C9 C10 1.507(6) . ?
C10 C11 1.412(6) . ?
C11 C12 1.353(7) . ?
C12 C13 1.405(7) . ?
C13 C14 1.400(7) . ?
C13 C18 1.422(6) . ?
C14 C15 1.368(7) . ?
C15 C16 1.405(6) . ?
C16 C17 1.371(7) . ?
C17 C18 1.418(7) . ?
C19 C20 1.515(7) . ?
C20 C21 1.412(6) . ?
C21 C22 1.355(7) . ?
C22 C23 1.411(6) . ?
C23 C24 1.403(7) . ?
C23 C28 1.428(6) . ?
C24 C25 1.367(6) . ?
C25 C26 1.399(6) . ?
C26 C27 1.390(6) . ?
C27 C28 1.421(6) . ?

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
O2B Cl1 O4B 106.4(9) . . ?
O1A Cl1 O4A 101.4(9) . . ?
O4C Cl1 O2C 115.5(8) . . ?
O1A Cl1 O3A 109.6(9) . . ?
O4A Cl1 O3A 111.3(9) . . ?
O1A Cl1 O2A 113.3(14) . . ?
O4A Cl1 O2A 105.6(17) . . ?
O3A Cl1 O2A 114.8(12) . . ?
O2B Cl1 O3B 124.7(8) . . ?
O4B Cl1 O3B 105.9(8) . . ?
O4C Cl1 O3C 108.6(13) . . ?
O2C Cl1 O3C 118.1(12) . . ?
O2B Cl1 O1B 112.3(7) . . ?
O4B Cl1 O1B 103.4(11) . . ?
O3B Cl1 O1B 102.2(7) . . ?
O4C Cl1 O1C 102.4(8) . . ?
O2C Cl1 O1C 96.7(8) . . ?
O3C Cl1 O1C 114.0(8) . . ?
N3 Pb1 O2 78.49(12) . . ?
N3 Pb1 N6 77.20(12) . . ?
O2 Pb1 N6 64.98(10) . . ?
N3 Pb1 N4 70.39(11) . . ?
O2 Pb1 N4 122.97(10) . . ?
N6 Pb1 N4 62.27(12) . . ?
N3 Pb1 N2 69.09(11) . . ?
O2 Pb1 N2 95.61(10) . . ?
N6 Pb1 N2 144.05(10) . . ?
N4 Pb1 N2 114.88(12) . . ?
N3 Pb1 N1 86.31(13) . . ?
O2 Pb1 N1 158.15(11) . . ?
N6 Pb1 N1 126.86(11) . . ?
N4 Pb1 N1 64.59(11) . . ?
N2 Pb1 N1 64.04(11) . . ?
C1 N1 C8 113.6(4) . . ?
C1 N1 Pb1 116.8(3) . . ?
C8 N1 Pb1 116.3(3) . . ?
C9 N2 C2 109.0(3) . . ?
C9 N2 C3 108.3(3) . . ?
C2 N2 C3 112.1(4) . . ?
C9 N2 Pb1 111.7(3) . . ?
C2 N2 Pb1 108.4(2) . . ?
C3 N2 Pb1 107.3(2) . . ?
C5 N3 C4 113.7(4) . . ?
C5 N3 Pb1 113.0(3) . . ?
C4 N3 Pb1 112.1(3) . . ?
C19 N4 C7 108.3(3) . . ?
C19 N4 C6 109.4(3) . . ?
C7 N4 C6 112.5(4) . . ?
C19 N4 Pb1 109.6(3) . . ?
C7 N4 Pb1 110.2(3) . . ?
C6 N4 Pb1 106.7(2) . . ?
C10 N5 C18 118.7(4) . . ?
C20 N6 C28 120.4(4) . . ?
C20 N6 Pb1 122.0(3) . . ?
C28 N6 Pb1 117.5(3) . . ?
C27 O2 Pb1 119.6(3) . . ?
N1 C1 C2 110.4(4) . . ?
N2 C2 C1 114.0(3) . . ?
N2 C3 C4 110.7(4) . . ?
N3 C4 C3 110.9(3) . . ?
N3 C5 C6 112.4(4) . . ?
N4 C6 C5 114.3(4) . . ?
N4 C7 C8 114.2(4) . . ?
N1 C8 C7 110.6(4) . . ?
N2 C9 C10 114.6(3) . . ?
N5 C10 C11 121.7(5) . . ?
N5 C10 C9 116.8(4) . . ?
C11 C10 C9 121.5(4) . . ?
C12 C11 C10 120.2(5) . . ?
C11 C12 C13 120.0(4) . . ?
C14 C13 C12 124.6(4) . . ?
C14 C13 C18 119.4(5) . . ?
C12 C13 C18 115.9(4) . . ?
C15 C14 C13 119.9(5) . . ?
C14 C15 C16 121.5(5) . . ?
C17 C16 C15 119.8(5) . . ?
O1 C17 C16 119.3(5) . . ?
O1 C17 C18 120.5(4) . . ?
C16 C17 C18 120.1(4) . . ?
N5 C18 C17 117.1(4) . . ?
N5 C18 C13 123.5(5) . . ?
C17 C18 C13 119.2(5) . . ?
N4 C19 C20 110.9(3) . . ?
N6 C20 C21 121.0(5) . . ?
N6 C20 C19 117.4(4) . . ?
C21 C20 C19 121.6(4) . . ?
C22 C21 C20 119.6(4) . . ?
C21 C22 C23 121.0(4) . . ?
C24 C23 C22 124.8(4) . . ?
C24 C23 C28 118.9(4) . . ?
C22 C23 C28 116.3(4) . . ?
C25 C24 C23 119.7(4) . . ?
C24 C25 C26 121.6(5) . . ?
C27 C26 C25 121.5(4) . . ?
O2 C27 C26 122.5(4) . . ?
O2 C27 C28 120.3(4) . . ?
C26 C27 C28 117.2(4) . . ?
N6 C28 C27 117.2(4) . . ?
N6 C28 C23 121.6(4) . . ?
C27 C28 C23 121.2(4) . . ?

_refine_diff_density_max         1.410
_refine_diff_density_min         -1.239
_refine_diff_density_rms         0.151



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_CdL4-ClO4-H2O
_database_code_depnum_ccdc_archive 'CCDC 2375280'
loop_
_audit_author_name
_audit_author_address
'Patrizia Rossi'
;University of Firenze
Italy
;
_audit_update_record             
;
2024-08-02 deposited with the CCDC.	2024-12-11 downloaded from the CCDC.
;

# start Validation Reply Form

_vrf_PLAT417_CdL4-ClO4-H2O       
;
PROBLEM: Short Inter D-H..H-D H1WB ..H2O . 1.94 Ang.
RESPONSE: H1wb and the oxygen atom O2 are involved in a strong 
hydrogen bond
;
_vrf_PLAT910_CdL4-ClO4-H2O       
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min). 21 Note
RESPONSE: this is probably due to the beamstop mask
;
# end Validation Reply Form

_publ_section_title_             
;
Zn(II)/Cd(II) selective binding and fluorescence sensing 
by using macrocyclic tetra-amines with different fluorophores. 
Clues for design of selective chemosensors for transition metals.
;
_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H36 Cd Cl2 N6 O11'
_chemical_formula_weight         815.93

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'

_cell_length_a                   11.0170(4)
_cell_length_b                   14.7346(5)
_cell_length_c                   19.6206(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3185.0(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4998
_cell_measurement_theta_min      4.1462
_cell_measurement_theta_max      26.6902

_exptl_crystal_description       prism
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.702
_exptl_crystal_F_000             1664
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.21
_exptl_absorpt_coefficient_mu    0.924
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.81413
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15908
_diffrn_reflns_av_unetI/netI     0.0929
_diffrn_reflns_av_R_equivalents  0.0630
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         4.155
_diffrn_reflns_theta_max         26.748
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.860
_diffrn_measured_fraction_theta_full 0.963
_diffrn_reflns_Laue_measured_fraction_max 0.860
_diffrn_reflns_Laue_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.823
_diffrn_reflns_point_group_measured_fraction_full 0.944
_reflns_number_total             5563
_reflns_number_gt                4051
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.709
_reflns_Friedel_fraction_max     0.775
_reflns_Friedel_fraction_full    0.920

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_cell_refinement       
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_data_reduction        
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_structure_solution    'SIR2004 (burla, 2005)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Mercury 3.10.1'
_computing_publication_material  'PARST(Nardelli, 1995)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0330P)²+2.4206P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1331 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.06(2)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5563
_refine_ls_number_parameters     445
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0845
_refine_ls_R_factor_gt           0.0489
_refine_ls_wR_factor_ref         0.1035
_refine_ls_wR_factor_gt          0.0845
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_restrained_S_all      1.007
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
Cd1 Cd 0.63370(6) 0.95268(4) 0.73583(3) 0.0349(2) Uani 1 1 d . . . . .
O1 O 0.7376(5) 1.1182(4) 0.7491(3) 0.0433(17) Uani 1 1 d D . . . .
H1O H 0.790(4) 1.136(5) 0.777(2) 0.052 Uiso 1 1 d D U . . .
O2 O 0.4072(5) 1.0032(4) 0.7207(3) 0.0431(17) Uani 1 1 d D . . . .
H2O H 0.357(4) 0.988(5) 0.690(2) 0.052 Uiso 1 1 d D U . . .
N3 N 0.5347(7) 0.8116(5) 0.7591(4) 0.042(2) Uani 1 1 d . . . . .
H3 H 0.463530 0.825247 0.787222 0.050 Uiso 1 1 calc R U . . .
N2 N 0.6324(9) 0.8674(5) 0.6294(4) 0.045(2) Uani 1 1 d . . . . .
N1 N 0.8406(7) 0.9325(5) 0.7098(4) 0.046(2) Uani 1 1 d . . . . .
H1 H 0.866496 0.987029 0.685186 0.055 Uiso 1 1 calc R U . . .
N4 N 0.7345(7) 0.8894(5) 0.8391(4) 0.043(2) Uani 1 1 d . . . . .
N5 N 0.6267(7) 1.0532(5) 0.6388(3) 0.0349(17) Uani 1 1 d . . . . .
N6 N 0.5346(7) 1.0043(5) 0.8358(4) 0.0325(18) Uani 1 1 d . . . . .
C4 C 0.4907(9) 0.7708(7) 0.6968(5) 0.045(3) Uani 1 1 d . . . . .
H4A H 0.418965 0.803051 0.681440 0.054 Uiso 1 1 calc R U . . .
H4B H 0.467866 0.708278 0.705518 0.054 Uiso 1 1 calc R U . . .
C3 C 0.5871(9) 0.7735(6) 0.6410(5) 0.047(3) Uani 1 1 d . . . . .
H3A H 0.654402 0.734693 0.653915 0.057 Uiso 1 1 calc R U . . .
H3B H 0.552907 0.750025 0.599009 0.057 Uiso 1 1 calc R U . . .
C2 C 0.7616(10) 0.8667(7) 0.6057(6) 0.053(3) Uani 1 1 d . . . . .
H2A H 0.772439 0.817111 0.573812 0.064 Uiso 1 1 calc R U . . .
H2B H 0.777886 0.922829 0.581568 0.064 Uiso 1 1 calc R U . . .
C1 C 0.8513(10) 0.8568(7) 0.6618(6) 0.059(3) Uani 1 1 d . . . . .
H1B H 0.837286 0.800064 0.685623 0.071 Uiso 1 1 calc R U . . .
H1A H 0.932666 0.855417 0.643052 0.071 Uiso 1 1 calc R U . . .
C8 C 0.9147(8) 0.9269(7) 0.7700(6) 0.055(3) Uani 1 1 d . . . . .
H8A H 0.923818 0.987169 0.789285 0.066 Uiso 1 1 calc R U . . .
H8B H 0.994735 0.905178 0.757539 0.066 Uiso 1 1 calc R U . . .
C7 C 0.8606(10) 0.8635(7) 0.8244(5) 0.052(3) Uani 1 1 d . . . . .
H7B H 0.862993 0.801337 0.808115 0.062 Uiso 1 1 calc R U . . .
H7A H 0.908582 0.867073 0.865717 0.062 Uiso 1 1 calc R U . . .
C6 C 0.6633(9) 0.8074(6) 0.8618(5) 0.051(3) Uani 1 1 d . . . . .
H6B H 0.714700 0.768552 0.889368 0.061 Uiso 1 1 calc R U . . .
H6A H 0.595166 0.826585 0.889545 0.061 Uiso 1 1 calc R U . . .
C5 C 0.6174(10) 0.7548(6) 0.8012(5) 0.052(3) Uani 1 1 d . . . . .
H5A H 0.685589 0.735112 0.773608 0.062 Uiso 1 1 calc R U . . .
H5B H 0.574411 0.701233 0.816729 0.062 Uiso 1 1 calc R U . . .
C9 C 0.5533(10) 0.9158(6) 0.5818(5) 0.049(3) Uani 1 1 d . . . . .
H9A H 0.469336 0.902498 0.592702 0.059 Uiso 1 1 calc R U . . .
H9B H 0.568861 0.894404 0.535870 0.059 Uiso 1 1 calc R U . . .
C10 C 0.5731(9) 1.0188(7) 0.5844(5) 0.044(3) Uani 1 1 d . . . . .
C11 C 0.5395(10) 1.0729(7) 0.5286(5) 0.051(3) Uani 1 1 d . . . . .
H11 H 0.498483 1.047531 0.491826 0.061 Uiso 1 1 calc R U . . .
C12 C 0.5675(10) 1.1629(7) 0.5289(5) 0.051(3) Uani 1 1 d . . . . .
H12 H 0.545133 1.199290 0.492328 0.061 Uiso 1 1 calc R U . . .
C13 C 0.6302(10) 1.2009(6) 0.5844(4) 0.041(2) Uani 1 1 d . . . . .
C14 C 0.6720(9) 1.2919(6) 0.5872(5) 0.042(3) Uani 1 1 d . . . . .
H14 H 0.655533 1.331280 0.551386 0.050 Uiso 1 1 calc R U . . .
C15 C 0.7347(10) 1.3212(6) 0.6409(5) 0.044(3) Uani 1 1 d . . . . .
H15 H 0.763335 1.380543 0.641204 0.053 Uiso 1 1 calc R U . . .
C16 C 0.7591(9) 1.2644(6) 0.6974(5) 0.042(3) Uani 1 1 d . . . . .
H16 H 0.801844 1.286467 0.734798 0.050 Uiso 1 1 calc R U . . .
C17 C 0.7195(8) 1.1777(6) 0.6964(5) 0.032(2) Uani 1 1 d . . . . .
C18 C 0.6563(8) 1.1436(6) 0.6401(4) 0.034(2) Uani 1 1 d . . . . .
C19 C 0.7247(9) 0.9619(7) 0.8893(5) 0.049(3) Uani 1 1 d . . . . .
H19A H 0.779615 1.010718 0.877204 0.058 Uiso 1 1 calc R U . . .
H19B H 0.748524 0.938969 0.933696 0.058 Uiso 1 1 calc R U . . .
C20 C 0.5962(9) 0.9983(6) 0.8931(5) 0.040(3) Uani 1 1 d . . . . .
C21 C 0.5468(10) 1.0239(7) 0.9563(5) 0.049(3) Uani 1 1 d . . . . .
H21 H 0.593758 1.021428 0.995611 0.059 Uiso 1 1 calc R U . . .
C22 C 0.4312(10) 1.0518(7) 0.9592(5) 0.050(3) Uani 1 1 d . . . . .
H22 H 0.398299 1.068979 1.000903 0.060 Uiso 1 1 calc R U . . .
C23 C 0.3584(9) 1.0557(6) 0.9001(5) 0.040(2) Uani 1 1 d . . . . .
C24 C 0.2362(10) 1.0817(6) 0.8992(6) 0.051(3) Uani 1 1 d . . . . .
H24 H 0.197783 1.098650 0.939490 0.061 Uiso 1 1 calc R U . . .
C25 C 0.1730(10) 1.0822(6) 0.8387(6) 0.051(3) Uani 1 1 d . . . . .
H25 H 0.092195 1.100565 0.838326 0.062 Uiso 1 1 calc R U . . .
C26 C 0.2278(8) 1.0559(6) 0.7784(5) 0.045(2) Uani 1 1 d . . . . .
H26 H 0.182961 1.055455 0.738238 0.054 Uiso 1 1 calc R U . . .
C27 C 0.3483(8) 1.0301(5) 0.7772(5) 0.034(2) Uani 1 1 d . . . . .
C28 C 0.4156(8) 1.0306(6) 0.8386(5) 0.034(2) Uani 1 1 d . . . . .
Cl1 Cl 1.0164(2) 1.12572(18) 0.61220(14) 0.0488(7) Uani 1 1 d . . . . .
O11 O 0.9323(7) 1.1682(6) 0.5697(4) 0.090(3) Uani 1 1 d . . . . .
O12 O 0.9975(7) 1.0300(5) 0.6121(4) 0.078(3) Uani 1 1 d . . . . .
O13 O 1.0092(7) 1.1565(5) 0.6811(4) 0.069(2) Uani 1 1 d . . . . .
O14 O 1.1358(7) 1.1413(5) 0.5857(4) 0.065(2) Uani 1 1 d . . . . .
Cl2 Cl 0.8407(3) 1.23732(19) 0.90382(14) 0.0563(8) Uani 1 1 d . . . . .
O21 O 0.8772(9) 1.1725(5) 0.8547(4) 0.090(3) Uani 1 1 d . . . . .
O22 O 0.9305(9) 1.2479(6) 0.9537(4) 0.096(3) Uani 1 1 d . . . . .
O23 O 0.8303(9) 1.3213(5) 0.8676(4) 0.088(3) Uani 1 1 d . . . . .
O24 O 0.7282(10) 1.2142(9) 0.9310(6) 0.145(5) Uani 1 1 d . . . . .
O1W O 0.2807(7) 0.9884(5) 0.6091(4) 0.066(2) Uani 1 1 d D . . . .
H1WA H 0.237(5) 1.035(2) 0.611(5) 0.079 Uiso 1 1 d D U . . .
H1WB H 0.239(5) 0.945(3) 0.624(4) 0.079 Uiso 1 1 d D U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Cd1 N1 2.355(7) . ?
Cd1 N6 2.371(7) . ?
Cd1 N3 2.392(7) . ?
Cd1 N5 2.413(6) . ?
Cd1 N2 2.438(7) . ?
Cd1 N4 2.492(8) . ?
Cd1 O2 2.621(6) . ?
O1 C17 1.370(10) . ?
O2 C27 1.344(10) . ?
N3 C4 1.446(12) . ?
N3 C5 1.487(12) . ?
N2 C9 1.463(12) . ?
N2 C3 1.489(11) . ?
N2 C2 1.496(13) . ?
N1 C8 1.440(12) . ?
N1 C1 1.463(12) . ?
N4 C19 1.456(12) . ?
N4 C7 1.470(13) . ?
N4 C6 1.508(11) . ?
N5 C10 1.321(11) . ?
N5 C18 1.371(11) . ?
N6 C20 1.317(11) . ?
N6 C28 1.367(11) . ?
C4 C3 1.525(13) . ?
C2 C1 1.486(15) . ?
C8 C7 1.537(13) . ?
C6 C5 1.507(13) . ?
C9 C10 1.533(13) . ?
C10 C11 1.405(13) . ?
C11 C12 1.361(13) . ?
C12 C13 1.405(13) . ?
C13 C18 1.411(11) . ?
C13 C14 1.419(13) . ?
C14 C15 1.331(13) . ?
C15 C16 1.416(13) . ?
C16 C17 1.350(12) . ?
C17 C18 1.399(12) . ?
C19 C20 1.516(13) . ?
C20 C21 1.405(13) . ?
C21 C22 1.340(13) . ?
C22 C23 1.410(12) . ?
C23 C24 1.401(14) . ?
C23 C28 1.411(11) . ?
C24 C25 1.377(14) . ?
C25 C26 1.384(13) . ?
C26 C27 1.380(12) . ?
C27 C28 1.415(11) . ?
Cl1 O11 1.395(7) . ?
Cl1 O12 1.426(8) . ?
Cl1 O13 1.428(7) . ?
Cl1 O14 1.433(7) . ?
Cl2 O24 1.392(10) . ?
Cl2 O22 1.400(8) . ?
Cl2 O21 1.415(8) . ?
Cl2 O23 1.431(8) . ?

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 Cd1 N6 131.8(3) . . ?
N1 Cd1 N3 111.9(3) . . ?
N6 Cd1 N3 84.9(3) . . ?
N1 Cd1 N5 86.4(3) . . ?
N6 Cd1 N5 116.1(2) . . ?
N3 Cd1 N5 132.0(3) . . ?
N1 Cd1 N2 75.8(3) . . ?
N6 Cd1 N2 150.7(3) . . ?
N3 Cd1 N2 73.3(3) . . ?
N5 Cd1 N2 68.9(2) . . ?
N1 Cd1 N4 72.4(3) . . ?
N6 Cd1 N4 69.7(3) . . ?
N3 Cd1 N4 73.9(3) . . ?
N5 Cd1 N4 152.3(3) . . ?
N2 Cd1 N4 120.4(3) . . ?
N1 Cd1 O2 158.9(2) . . ?
N6 Cd1 O2 64.2(2) . . ?
N3 Cd1 O2 80.5(2) . . ?
N5 Cd1 O2 72.9(2) . . ?
N2 Cd1 O2 92.5(3) . . ?
N4 Cd1 O2 128.5(2) . . ?
C27 O2 Cd1 116.7(5) . . ?
C4 N3 C5 116.2(7) . . ?
C4 N3 Cd1 110.7(6) . . ?
C5 N3 Cd1 108.4(6) . . ?
C9 N2 C3 110.6(8) . . ?
C9 N2 C2 111.8(8) . . ?
C3 N2 C2 111.2(7) . . ?
C9 N2 Cd1 107.3(5) . . ?
C3 N2 Cd1 110.4(6) . . ?
C2 N2 Cd1 105.3(6) . . ?
C8 N1 C1 116.0(8) . . ?
C8 N1 Cd1 112.2(5) . . ?
C1 N1 Cd1 108.3(6) . . ?
C19 N4 C7 113.2(8) . . ?
C19 N4 C6 110.5(8) . . ?
C7 N4 C6 109.9(7) . . ?
C19 N4 Cd1 104.1(5) . . ?
C7 N4 Cd1 111.0(6) . . ?
C6 N4 Cd1 107.9(6) . . ?
C10 N5 C18 119.6(8) . . ?
C10 N5 Cd1 114.6(6) . . ?
C18 N5 Cd1 125.0(6) . . ?
C20 N6 C28 118.6(8) . . ?
C20 N6 Cd1 116.6(6) . . ?
C28 N6 Cd1 124.4(6) . . ?
N3 C4 C3 111.2(8) . . ?
N2 C3 C4 111.6(8) . . ?
C1 C2 N2 113.8(8) . . ?
N1 C1 C2 110.3(9) . . ?
N1 C8 C7 112.6(8) . . ?
N4 C7 C8 110.2(8) . . ?
C5 C6 N4 110.7(8) . . ?
N3 C5 C6 110.8(8) . . ?
N2 C9 C10 112.1(9) . . ?
N5 C10 C11 122.0(9) . . ?
N5 C10 C9 118.1(9) . . ?
C11 C10 C9 119.9(10) . . ?
C12 C11 C10 119.3(10) . . ?
C11 C12 C13 120.2(9) . . ?
C12 C13 C18 117.5(9) . . ?
C12 C13 C14 124.5(9) . . ?
C18 C13 C14 118.0(9) . . ?
C15 C14 C13 120.4(9) . . ?
C14 C15 C16 121.8(9) . . ?
C17 C16 C15 119.1(10) . . ?
C16 C17 O1 123.1(9) . . ?
C16 C17 C18 120.8(9) . . ?
O1 C17 C18 116.0(7) . . ?
N5 C18 C17 118.8(8) . . ?
N5 C18 C13 121.2(8) . . ?
C17 C18 C13 119.9(8) . . ?
N4 C19 C20 111.2(8) . . ?
N6 C20 C21 122.4(9) . . ?
N6 C20 C19 117.6(9) . . ?
C21 C20 C19 120.0(9) . . ?
C22 C21 C20 119.2(9) . . ?
C21 C22 C23 121.2(9) . . ?
C24 C23 C28 119.4(9) . . ?
C24 C23 C22 124.6(9) . . ?
C28 C23 C22 116.0(9) . . ?
C25 C24 C23 119.9(10) . . ?
C24 C25 C26 121.0(10) . . ?
C25 C26 C27 120.8(9) . . ?
O2 C27 C26 124.0(8) . . ?
O2 C27 C28 116.8(7) . . ?
C26 C27 C28 119.2(8) . . ?
N6 C28 C23 122.4(9) . . ?
N6 C28 C27 117.9(8) . . ?
C23 C28 C27 119.7(8) . . ?
O11 Cl1 O12 110.2(6) . . ?
O11 Cl1 O13 112.7(5) . . ?
O12 Cl1 O13 107.9(5) . . ?
O11 Cl1 O14 108.8(5) . . ?
O12 Cl1 O14 107.0(5) . . ?
O13 Cl1 O14 110.1(5) . . ?
O24 Cl2 O22 112.9(7) . . ?
O24 Cl2 O21 110.4(7) . . ?
O22 Cl2 O21 110.5(6) . . ?
O24 Cl2 O23 109.3(7) . . ?
O22 Cl2 O23 107.9(5) . . ?
O21 Cl2 O23 105.6(5) . . ?

_refine_diff_density_max         0.768
_refine_diff_density_min         -0.746
_refine_diff_density_rms         0.099



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_ZnL3-ClO4-05H2O
_database_code_depnum_ccdc_archive 'CCDC 2375279'
loop_
_audit_author_name
_audit_author_address
'Patrizia Rossi'
;University of Firenze
Italy
;
_audit_update_record             
;
2024-08-02 deposited with the CCDC.	2024-12-11 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT430_ZnL3-ClO4-05H2O     
;
PROBLEM: Short Inter D...A Contact O1W ..O22B . 2.45 Ang.
RESPONSE: between O1w and O22b, probably, there is a
hydrogen-bond. The hydrogen atoms of the water molecule were
not introduced in the refinement
;
_vrf_PLAT910_ZnL3-ClO4-05H2O     
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min). 27 Note
RESPONSE: this is probably due to the beamstop mask
;
# end Validation Reply Form

_publ_section_title_             
;
Zn(II)/Cd(II) selective binding and fluorescence sensing 
by using macrocyclic tetra-amines with different fluorophores. 
Clues for design of selective chemosensors for transition metals.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H35 Cl2 N6 O8.50 Zn'
_chemical_formula_weight         727.89

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   10.5259(4)
_cell_length_b                   17.3495(6)
_cell_length_c                   16.8877(6)
_cell_angle_alpha                90
_cell_angle_beta                 96.977(3)
_cell_angle_gamma                90
_cell_volume                     3061.18(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    7068
_cell_measurement_theta_min      4.2163
_cell_measurement_theta_max      29.3684

_exptl_crystal_description       prism
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_F_000             1508
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_exptl_absorpt_coefficient_mu    1.039
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.83766
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_detector_area_resol_mean 16.4547
_diffrn_reflns_number            24336
_diffrn_reflns_av_unetI/netI     0.0502
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         4.275
_diffrn_reflns_theta_max         29.433
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.861
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.861
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.861
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             7298
_reflns_number_gt                5479
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_cell_refinement       
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_data_reduction        
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_structure_solution    'SIR2004 (Burla, 2005)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Mercury 3.10.1'
_computing_publication_material  'PARST(Nardelli, 1995)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0507P)²+5.6088P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7298
_refine_ls_number_parameters     431
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0842
_refine_ls_R_factor_gt           0.0590
_refine_ls_wR_factor_ref         0.1448
_refine_ls_wR_factor_gt          0.1326
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_restrained_S_all      1.070
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
Zn1 Zn 0.38042(4) 0.12861(2) 0.78364(2) 0.02744(12) Uani 1 1 d . . . . .
Cl1 Cl 0.72816(9) 0.14545(5) 0.07807(6) 0.0393(2) Uani 1 1 d . . . . .
O11 O 0.6409(3) 0.2015(2) 0.0981(3) 0.0925(15) Uani 1 1 d . . . . .
O12 O 0.6604(3) 0.07475(16) 0.05993(18) 0.0524(8) Uani 1 1 d . . . . .
O13 O 0.7889(3) 0.1706(2) 0.0118(2) 0.0706(10) Uani 1 1 d . . . . .
O14 O 0.8245(3) 0.1358(2) 0.1425(2) 0.0637(9) Uani 1 1 d . . . . .
Cl2 Cl 0.71928(9) 0.48268(6) 0.87556(6) 0.0417(2) Uani 1 1 d . . . . .
O21A O 0.7229(9) 0.4436(6) 0.7975(6) 0.046(2) Uiso 0.487(9) 1 d . . P A 1
O22A O 0.8308(10) 0.5294(6) 0.8926(6) 0.067(3) Uiso 0.487(9) 1 d . . P A 1
O23A O 0.7238(6) 0.4184(4) 0.9280(4) 0.050(2) Uiso 0.487(9) 1 d . . P A 1
O24A O 0.6089(8) 0.5243(5) 0.8829(6) 0.070(3) Uiso 0.487(9) 1 d . . P A 1
O21B O 0.6956(19) 0.4607(11) 0.7938(11) 0.058(6) Uiso 0.254(12) 1 d . . P A 2
O22B O 0.6472(15) 0.5540(8) 0.8509(9) 0.047(4) Uiso 0.254(12) 1 d . . P A 2
O23B O 0.6669(18) 0.4560(11) 0.9395(9) 0.068(6) Uiso 0.254(12) 1 d . . P A 2
O24B O 0.8547(11) 0.5086(8) 0.8983(8) 0.021(3) Uiso 0.254(12) 1 d . . P A 2
O21C O 0.6966(17) 0.4237(10) 0.8224(11) 0.068(5) Uiso 0.260(11) 1 d . . P A 3
O22C O 0.6076(15) 0.4899(9) 0.9292(9) 0.061(5) Uiso 0.260(11) 1 d . . P A 3
O23C O 0.706(3) 0.5585(13) 0.8425(13) 0.106(8) Uiso 0.260(11) 1 d . . P A 3
O24C O 0.8411(17) 0.4855(12) 0.9237(12) 0.076(6) Uiso 0.260(11) 1 d . . P A 3
N1 N 0.5069(3) 0.03320(17) 0.82667(19) 0.0327(7) Uani 1 1 d . . . . .
H1N H 0.481(4) 0.011(2) 0.868(3) 0.039 Uiso 1 1 d . U . . .
N2 N 0.5708(3) 0.18609(17) 0.79196(19) 0.0353(7) Uani 1 1 d . . . . .
N3 N 0.3611(3) 0.18126(19) 0.6669(2) 0.0391(8) Uani 1 1 d . . . . .
H3N H 0.326(4) 0.228(3) 0.668(3) 0.047 Uiso 1 1 d . U . . .
N4 N 0.2845(3) 0.03511(17) 0.70884(19) 0.0360(7) Uani 1 1 d . . . . .
N5 N 0.3527(3) 0.24165(16) 0.84142(18) 0.0315(7) Uani 1 1 d . . . . .
N6 N 0.2379(3) 0.08389(16) 0.85365(19) 0.0314(7) Uani 1 1 d . . . . .
C1 C 0.6376(4) 0.0591(2) 0.8492(3) 0.0394(9) Uani 1 1 d . . . . .
H1A H 0.697498 0.015913 0.844114 0.047 Uiso 1 1 calc R U . . .
H1B H 0.648085 0.076041 0.905651 0.047 Uiso 1 1 calc R U . . .
C2 C 0.6694(4) 0.1261(2) 0.7958(3) 0.0425(9) Uani 1 1 d . . . . .
H2A H 0.753168 0.148460 0.816957 0.051 Uiso 1 1 calc R U . . .
H2B H 0.676060 0.106538 0.741340 0.051 Uiso 1 1 calc R U . . .
C3 C 0.5683(4) 0.2328(2) 0.7189(3) 0.0462(10) Uani 1 1 d . . . . .
H3A H 0.657122 0.241854 0.707374 0.055 Uiso 1 1 calc R U . . .
H3B H 0.529171 0.283541 0.727531 0.055 Uiso 1 1 calc R U . . .
C4 C 0.4932(4) 0.1935(2) 0.6478(2) 0.0421(10) Uani 1 1 d . . . . .
H4A H 0.492125 0.226200 0.599671 0.050 Uiso 1 1 calc R U . . .
H4B H 0.533131 0.143495 0.637223 0.050 Uiso 1 1 calc R U . . .
C5 C 0.2810(5) 0.1357(2) 0.6073(3) 0.0472(10) Uani 1 1 d . . . . .
H5A H 0.304298 0.147138 0.553522 0.057 Uiso 1 1 calc R U . . .
H5B H 0.189960 0.149697 0.608140 0.057 Uiso 1 1 calc R U . . .
C6 C 0.2993(4) 0.0496(2) 0.6251(2) 0.0433(10) Uani 1 1 d . . . . .
H6A H 0.235209 0.019421 0.590226 0.052 Uiso 1 1 calc R U . . .
H6B H 0.385658 0.033321 0.614205 0.052 Uiso 1 1 calc R U . . .
C7 C 0.3494(4) -0.0370(2) 0.7375(2) 0.0404(9) Uani 1 1 d . . . . .
H7A H 0.338141 -0.076110 0.694552 0.049 Uiso 1 1 calc R U . . .
H7B H 0.309544 -0.057044 0.783485 0.049 Uiso 1 1 calc R U . . .
C8 C 0.4911(4) -0.0239(2) 0.7624(2) 0.0393(9) Uani 1 1 d . . . . .
H8A H 0.532568 -0.072962 0.780984 0.047 Uiso 1 1 calc R U . . .
H8B H 0.532229 -0.005193 0.716274 0.047 Uiso 1 1 calc R U . . .
C9 C 0.5840(4) 0.2348(2) 0.8625(3) 0.0403(9) Uani 1 1 d . . . . .
H9A H 0.643900 0.277380 0.854743 0.048 Uiso 1 1 calc R U . . .
H9B H 0.621802 0.204110 0.908877 0.048 Uiso 1 1 calc R U . . .
C10 C 0.4596(4) 0.2684(2) 0.8807(2) 0.0369(9) Uani 1 1 d . . . . .
C11 C 0.4601(5) 0.3239(2) 0.9415(3) 0.0476(10) Uani 1 1 d . . . . .
H11 H 0.538656 0.344069 0.966677 0.057 Uiso 1 1 calc R U . . .
C12 C 0.3475(5) 0.3482(3) 0.9639(3) 0.0562(13) Uani 1 1 d . . . . .
H12 H 0.347333 0.383323 1.007040 0.067 Uiso 1 1 calc R U . . .
C13 C 0.2301(5) 0.3216(2) 0.9232(2) 0.0431(10) Uani 1 1 d . . . . .
C14 C 0.1085(6) 0.3456(3) 0.9405(3) 0.0584(14) Uani 1 1 d . . . . .
H14 H 0.102399 0.378776 0.984661 0.070 Uiso 1 1 calc R U . . .
C15 C 0.0017(5) 0.3226(3) 0.8959(4) 0.0635(15) Uani 1 1 d . . . . .
H15 H -0.079387 0.339017 0.908785 0.076 Uiso 1 1 calc R U . . .
C16 C 0.0093(4) 0.2744(2) 0.8302(3) 0.0547(13) Uani 1 1 d . . . . .
H16 H -0.067074 0.259199 0.798088 0.066 Uiso 1 1 calc R U . . .
C17 C 0.1257(4) 0.2485(2) 0.8112(3) 0.0391(9) Uani 1 1 d . . . . .
H17 H 0.129907 0.215899 0.766440 0.047 Uiso 1 1 calc R U . . .
C18 C 0.2375(4) 0.2709(2) 0.8589(2) 0.0341(8) Uani 1 1 d . . . . .
C19 C 0.1509(4) 0.0343(2) 0.7244(3) 0.0429(10) Uani 1 1 d . . . . .
H19A H 0.114601 -0.017621 0.712427 0.051 Uiso 1 1 calc R U . . .
H19B H 0.101541 0.071501 0.688339 0.051 Uiso 1 1 calc R U . . .
C20 C 0.1366(4) 0.0548(2) 0.8098(2) 0.0367(9) Uani 1 1 d . . . . .
C21 C 0.0173(4) 0.0451(2) 0.8392(3) 0.0442(10) Uani 1 1 d . . . . .
H21 H -0.053208 0.023459 0.806143 0.053 Uiso 1 1 calc R U . . .
C22 C 0.0047(4) 0.0665(2) 0.9140(3) 0.0433(10) Uani 1 1 d . . . . .
H22 H -0.076493 0.063507 0.933042 0.052 Uiso 1 1 calc R U . . .
C23 C 0.1138(4) 0.0941(2) 0.9655(2) 0.0361(9) Uani 1 1 d . . . . .
C24 C 0.1104(4) 0.1123(2) 1.0457(3) 0.0419(10) Uani 1 1 d . . . . .
H24 H 0.031520 0.110386 1.067627 0.050 Uiso 1 1 calc R U . . .
C25 C 0.2200(4) 0.1329(2) 1.0929(3) 0.0404(9) Uani 1 1 d . . . . .
H25 H 0.217332 0.143964 1.147780 0.048 Uiso 1 1 calc R U . . .
C26 C 0.3362(4) 0.1377(2) 1.0605(2) 0.0360(8) Uani 1 1 d . . . . .
H26 H 0.411957 0.152148 1.093569 0.043 Uiso 1 1 calc R U . . .
C27 C 0.3416(3) 0.1219(2) 0.9820(2) 0.0335(8) Uani 1 1 d . . . . .
H27 H 0.420792 0.125501 0.960577 0.040 Uiso 1 1 calc R U . . .
C28 C 0.2290(3) 0.09996(18) 0.9321(2) 0.0293(7) Uani 1 1 d . . . . .
O1W O 0.5785(8) 0.6888(5) 0.8356(5) 0.078(2) Uiso 0.5 1 d . . P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Zn1 N3 2.160(3) . ?
Zn1 N6 2.164(3) . ?
Zn1 N1 2.192(3) . ?
Zn1 N4 2.222(3) . ?
Zn1 N5 2.226(3) . ?
Zn1 N2 2.227(3) . ?
Cl1 O14 1.405(4) . ?
Cl1 O11 1.406(3) . ?
Cl1 O13 1.423(3) . ?
Cl1 O12 1.433(3) . ?
Cl2 O21C 1.362(16) . ?
Cl2 O23B 1.353(15) . ?
Cl2 O24A 1.387(8) . ?
Cl2 O23C 1.43(2) . ?
Cl2 O23A 1.421(7) . ?
Cl2 O21B 1.425(19) . ?
Cl2 O22A 1.426(9) . ?
Cl2 O24C 1.434(17) . ?
Cl2 O21A 1.487(9) . ?
Cl2 O24B 1.499(11) . ?
Cl2 O22B 1.484(14) . ?
Cl2 O22C 1.574(15) . ?
N1 C1 1.454(5) . ?
N1 C8 1.465(5) . ?
N2 C9 1.454(5) . ?
N2 C2 1.466(5) . ?
N2 C3 1.475(5) . ?
N3 C5 1.464(5) . ?
N3 C4 1.480(5) . ?
N4 C19 1.461(5) . ?
N4 C6 1.463(5) . ?
N4 C7 1.478(5) . ?
N5 C10 1.320(5) . ?
N5 C18 1.379(5) . ?
N6 C20 1.322(5) . ?
N6 C28 1.368(5) . ?
C1 C2 1.533(5) . ?
C3 C4 1.517(6) . ?
C5 C6 1.531(5) . ?
C7 C8 1.517(6) . ?
C9 C10 1.498(5) . ?
C10 C11 1.407(6) . ?
C11 C12 1.354(7) . ?
C12 C13 1.416(7) . ?
C13 C18 1.407(5) . ?
C13 C14 1.409(6) . ?
C14 C15 1.336(8) . ?
C15 C16 1.401(7) . ?
C16 C17 1.379(6) . ?
C17 C18 1.398(6) . ?
C19 C20 1.510(6) . ?
C20 C21 1.415(5) . ?
C21 C22 1.340(6) . ?
C22 C23 1.436(6) . ?
C23 C24 1.395(6) . ?
C23 C28 1.402(5) . ?
C24 C25 1.367(6) . ?
C25 C26 1.403(5) . ?
C26 C27 1.361(5) . ?
C27 C28 1.420(5) . ?

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
N3 Zn1 N6 130.98(13) . . ?
N3 Zn1 N1 127.44(12) . . ?
N6 Zn1 N1 88.94(11) . . ?
N3 Zn1 N4 78.70(12) . . ?
N6 Zn1 N4 75.60(12) . . ?
N1 Zn1 N4 81.54(12) . . ?
N3 Zn1 N5 91.41(12) . . ?
N6 Zn1 N5 86.55(11) . . ?
N1 Zn1 N5 128.82(12) . . ?
N4 Zn1 N5 144.87(12) . . ?
N3 Zn1 N2 81.50(13) . . ?
N6 Zn1 N2 143.54(12) . . ?
N1 Zn1 N2 79.15(11) . . ?
N4 Zn1 N2 134.92(12) . . ?
N5 Zn1 N2 75.09(11) . . ?
O14 Cl1 O11 109.1(3) . . ?
O14 Cl1 O13 107.1(2) . . ?
O11 Cl1 O13 110.3(3) . . ?
O14 Cl1 O12 110.91(19) . . ?
O11 Cl1 O12 108.7(2) . . ?
O13 Cl1 O12 110.7(2) . . ?
O21C Cl2 O23C 115.6(12) . . ?
O24A Cl2 O23A 108.6(5) . . ?
O23B Cl2 O21B 129.9(10) . . ?
O24A Cl2 O22A 111.3(6) . . ?
O23A Cl2 O22A 110.8(5) . . ?
O21C Cl2 O24C 118.2(10) . . ?
O23C Cl2 O24C 103.1(12) . . ?
O24A Cl2 O21A 115.4(5) . . ?
O23A Cl2 O21A 101.0(5) . . ?
O22A Cl2 O21A 109.2(5) . . ?
O23B Cl2 O24B 111.4(8) . . ?
O21B Cl2 O24B 112.2(9) . . ?
O23B Cl2 O22B 105.4(10) . . ?
O21B Cl2 O22B 85.9(10) . . ?
O24B Cl2 O22B 105.0(8) . . ?
O21C Cl2 O22C 110.8(10) . . ?
O23C Cl2 O22C 96.3(11) . . ?
O24C Cl2 O22C 110.5(10) . . ?
C1 N1 C8 115.0(3) . . ?
C1 N1 Zn1 111.8(2) . . ?
C8 N1 Zn1 104.8(2) . . ?
C9 N2 C2 112.4(3) . . ?
C9 N2 C3 110.9(3) . . ?
C2 N2 C3 111.6(3) . . ?
C9 N2 Zn1 107.9(2) . . ?
C2 N2 Zn1 108.2(2) . . ?
C3 N2 Zn1 105.6(2) . . ?
C5 N3 C4 113.9(3) . . ?
C5 N3 Zn1 112.4(3) . . ?
C4 N3 Zn1 105.9(2) . . ?
C19 N4 C6 113.2(3) . . ?
C19 N4 C7 110.5(3) . . ?
C6 N4 C7 111.2(3) . . ?
C19 N4 Zn1 106.6(2) . . ?
C6 N4 Zn1 109.2(2) . . ?
C7 N4 Zn1 105.8(2) . . ?
C10 N5 C18 118.8(3) . . ?
C10 N5 Zn1 112.4(2) . . ?
C18 N5 Zn1 125.7(2) . . ?
C20 N6 C28 118.4(3) . . ?
C20 N6 Zn1 113.3(3) . . ?
C28 N6 Zn1 126.1(2) . . ?
N1 C1 C2 110.3(3) . . ?
N2 C2 C1 111.1(3) . . ?
N2 C3 C4 111.7(3) . . ?
N3 C4 C3 107.8(3) . . ?
N3 C5 C6 110.1(3) . . ?
N4 C6 C5 109.3(3) . . ?
N4 C7 C8 111.4(3) . . ?
N1 C8 C7 109.0(3) . . ?
N2 C9 C10 113.3(3) . . ?
N5 C10 C11 122.3(4) . . ?
N5 C10 C9 118.2(3) . . ?
C11 C10 C9 119.4(4) . . ?
C12 C11 C10 119.5(4) . . ?
C11 C12 C13 120.3(4) . . ?
C18 C13 C14 118.8(5) . . ?
C18 C13 C12 116.8(4) . . ?
C14 C13 C12 124.4(4) . . ?
C15 C14 C13 121.2(5) . . ?
C14 C15 C16 120.1(4) . . ?
C17 C16 C15 121.0(5) . . ?
C16 C17 C18 119.1(4) . . ?
N5 C18 C17 118.3(3) . . ?
N5 C18 C13 121.9(4) . . ?
C17 C18 C13 119.8(4) . . ?
N4 C19 C20 112.3(3) . . ?
N6 C20 C21 122.6(4) . . ?
N6 C20 C19 117.2(3) . . ?
C21 C20 C19 120.2(4) . . ?
C22 C21 C20 119.5(4) . . ?
C21 C22 C23 120.0(4) . . ?
C24 C23 C28 120.0(4) . . ?
C24 C23 C22 123.4(4) . . ?
C28 C23 C22 116.6(4) . . ?
C25 C24 C23 120.4(4) . . ?
C24 C25 C26 120.1(4) . . ?
C27 C26 C25 120.6(4) . . ?
C26 C27 C28 120.1(3) . . ?
N6 C28 C23 122.6(3) . . ?
N6 C28 C27 118.6(3) . . ?
C23 C28 C27 118.7(3) . . ?

_refine_diff_density_max         0.617
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.082



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_CdL3-ClO4-H2O
_database_code_depnum_ccdc_archive 'CCDC 2375278'
loop_
_audit_author_name
_audit_author_address
'Patrizia Rossi'
;University of Firenze
Italy
;
_audit_update_record             
;
2024-10-17 deposited with the CCDC.	2024-12-11 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT910_CdL3-ClO4-H2O       
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min). 26 Note
RESPONSE: this is probably due to the beamstop mask
;
# end Validation Reply Form

_publ_section_title_             
;
Zn(II)/Cd(II) selective binding and fluorescence sensing 
by using macrocyclic tetra-amines with different fluorophores. 
Clues for design of selective chemosensors for transition metals.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H36 Cd Cl2 N6 O9'
_chemical_formula_weight         783.93

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   8.4798(2)
_cell_length_b                   16.0482(4)
_cell_length_c                   23.2856(6)
_cell_angle_alpha                90
_cell_angle_beta                 90.338(2)
_cell_angle_gamma                90
_cell_volume                     3168.78(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    13103
_cell_measurement_theta_min      4.1848
_cell_measurement_theta_max      29.3183

_exptl_crystal_description       prism
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.643
_exptl_crystal_F_000             1600
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.19
_exptl_absorpt_coefficient_mu    0.920
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.68079
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            23329
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         4.192
_diffrn_reflns_theta_max         29.317
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.857
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.857
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.857
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             7431
_reflns_number_gt                6269
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_cell_refinement       
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_data_reduction        
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_structure_solution    'SIR2004 (Burla, 2005)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Mercury 3.10.1'
_computing_publication_material  'PARST(Nardelli, 1995)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0262P)²+1.8631P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7431
_refine_ls_number_parameters     442
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0303
_refine_ls_wR_factor_ref         0.0695
_refine_ls_wR_factor_gt          0.0662
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_restrained_S_all      1.068
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

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
Cd1 Cd 0.82202(2) 0.80908(2) 0.86391(2) 0.01701(5) Uani 1 1 d . . . . .
N3 N 0.5496(2) 0.80611(12) 0.84342(9) 0.0229(4) Uani 1 1 d . . . . .
H3N H 0.516(3) 0.7618(17) 0.8486(11) 0.028 Uiso 1 1 d . U . . .
N2 N 0.7083(2) 0.86339(11) 0.94973(8) 0.0209(4) Uani 1 1 d . . . . .
N1 N 0.9457(2) 0.93789(11) 0.87683(8) 0.0195(4) Uani 1 1 d . . . . .
H1N H 1.041(3) 0.9342(15) 0.8721(10) 0.023 Uiso 1 1 d . U . . .
N4 N 0.7954(2) 0.87312(11) 0.77097(8) 0.0195(4) Uani 1 1 d . . . . .
N5 N 0.7946(2) 0.69948(11) 0.92931(8) 0.0192(4) Uani 1 1 d . . . . .
N6 N 1.0208(2) 0.75457(11) 0.80491(8) 0.0187(4) Uani 1 1 d . . . . .
C1 C 0.4773(3) 0.86601(14) 0.88313(10) 0.0255(5) Uani 1 1 d . . . . .
H1A H 0.361205 0.859946 0.881761 0.031 Uiso 1 1 calc R U . . .
H1B H 0.503883 0.923449 0.871043 0.031 Uiso 1 1 calc R U . . .
C2 C 0.5357(3) 0.85166(15) 0.94403(10) 0.0248(5) Uani 1 1 d . . . . .
H2A H 0.481312 0.890803 0.970143 0.030 Uiso 1 1 calc R U . . .
H2B H 0.508141 0.794282 0.955957 0.030 Uiso 1 1 calc R U . . .
C3 C 0.7511(3) 0.95229(14) 0.95530(10) 0.0241(5) Uani 1 1 d . . . . .
H3A H 0.740421 0.969494 0.995919 0.029 Uiso 1 1 calc R U . . .
H3B H 0.677092 0.986270 0.932052 0.029 Uiso 1 1 calc R U . . .
C4 C 0.9189(3) 0.96899(14) 0.93563(10) 0.0233(5) Uani 1 1 d . . . . .
H4A H 0.939559 1.029689 0.936809 0.028 Uiso 1 1 calc R U . . .
H4B H 0.993855 0.941514 0.962333 0.028 Uiso 1 1 calc R U . . .
C5 C 0.8804(3) 0.99275(13) 0.83162(10) 0.0222(5) Uani 1 1 d . . . . .
H5A H 0.939849 1.045840 0.830800 0.027 Uiso 1 1 calc R U . . .
H5B H 0.768707 1.005555 0.839980 0.027 Uiso 1 1 calc R U . . .
C6 C 0.8924(3) 0.94963(14) 0.77375(10) 0.0225(5) Uani 1 1 d . . . . .
H6A H 0.857632 0.988534 0.743214 0.027 Uiso 1 1 calc R U . . .
H6B H 1.004004 0.935062 0.766470 0.027 Uiso 1 1 calc R U . . .
C7 C 0.6274(3) 0.89156(14) 0.75987(10) 0.0231(5) Uani 1 1 d . . . . .
H7A H 0.610254 0.898427 0.718044 0.028 Uiso 1 1 calc R U . . .
H7B H 0.599142 0.944695 0.778812 0.028 Uiso 1 1 calc R U . . .
C8 C 0.5205(3) 0.82245(15) 0.78204(10) 0.0247(5) Uani 1 1 d . . . . .
H8A H 0.408911 0.838741 0.776326 0.030 Uiso 1 1 calc R U . . .
H8B H 0.539544 0.770885 0.759793 0.030 Uiso 1 1 calc R U . . .
C9 C 0.7704(3) 0.81357(14) 0.99773(10) 0.0235(5) Uani 1 1 d . . . . .
H9A H 0.702862 0.822005 1.031770 0.028 Uiso 1 1 calc R U . . .
H9B H 0.877851 0.833278 1.007585 0.028 Uiso 1 1 calc R U . . .
C10 C 0.7767(3) 0.72182(14) 0.98371(10) 0.0214(5) Uani 1 1 d . . . . .
C11 C 0.7693(3) 0.66290(16) 1.02877(11) 0.0321(6) Uani 1 1 d . . . . .
H11 H 0.756585 0.680807 1.067360 0.038 Uiso 1 1 calc R U . . .
C12 C 0.7804(4) 0.58060(17) 1.01632(11) 0.0397(7) Uani 1 1 d . . . . .
H12 H 0.778503 0.540601 1.046382 0.048 Uiso 1 1 calc R U . . .
C13 C 0.7947(3) 0.55410(15) 0.95845(11) 0.0333(6) Uani 1 1 d . . . . .
C14 C 0.7998(4) 0.46909(17) 0.94185(13) 0.0501(9) Uani 1 1 d . . . . .
H14 H 0.799262 0.426757 0.970362 0.060 Uiso 1 1 calc R U . . .
C15 C 0.8054(4) 0.44790(16) 0.88554(13) 0.0461(8) Uani 1 1 d . . . . .
H15 H 0.808195 0.390783 0.874884 0.055 Uiso 1 1 calc R U . . .
C16 C 0.8072(3) 0.50973(16) 0.84281(11) 0.0316(6) Uani 1 1 d . . . . .
H16 H 0.809161 0.494291 0.803436 0.038 Uiso 1 1 calc R U . . .
C17 C 0.8061(3) 0.59157(15) 0.85777(10) 0.0242(5) Uani 1 1 d . . . . .
H17 H 0.809846 0.632982 0.828652 0.029 Uiso 1 1 calc R U . . .
C18 C 0.7996(3) 0.61579(14) 0.91561(10) 0.0222(5) Uani 1 1 d . . . . .
C19 C 0.8588(3) 0.81535(14) 0.72827(10) 0.0232(5) Uani 1 1 d . . . . .
H19A H 0.889185 0.847297 0.693694 0.028 Uiso 1 1 calc R U . . .
H19B H 0.774800 0.775744 0.716830 0.028 Uiso 1 1 calc R U . . .
C20 C 1.0002(3) 0.76652(14) 0.74934(10) 0.0205(5) Uani 1 1 d . . . . .
C21 C 1.1009(3) 0.73089(14) 0.70806(10) 0.0237(5) Uani 1 1 d . . . . .
H21 H 1.083886 0.741541 0.668369 0.028 Uiso 1 1 calc R U . . .
C22 C 1.2221(3) 0.68132(14) 0.72518(10) 0.0247(5) Uani 1 1 d . . . . .
H22 H 1.289694 0.656892 0.697490 0.030 Uiso 1 1 calc R U . . .
C23 C 1.2474(3) 0.66620(14) 0.78413(10) 0.0213(5) Uani 1 1 d . . . . .
C24 C 1.3693(3) 0.61404(14) 0.80541(11) 0.0256(5) Uani 1 1 d . . . . .
H24 H 1.437723 0.586708 0.779304 0.031 Uiso 1 1 calc R U . . .
C25 C 1.3892(3) 0.60278(15) 0.86293(11) 0.0284(5) Uani 1 1 d . . . . .
H25 H 1.468858 0.566147 0.876750 0.034 Uiso 1 1 calc R U . . .
C26 C 1.2919(3) 0.64543(15) 0.90203(11) 0.0265(5) Uani 1 1 d . . . . .
H26 H 1.309204 0.639040 0.942132 0.032 Uiso 1 1 calc R U . . .
C27 C 1.1728(3) 0.69584(14) 0.88286(10) 0.0232(5) Uani 1 1 d . . . . .
H27 H 1.108259 0.724324 0.909671 0.028 Uiso 1 1 calc R U . . .
C28 C 1.1455(3) 0.70577(13) 0.82359(9) 0.0189(5) Uani 1 1 d . . . . .
O1W O 1.5427(3) 0.72953(15) 1.14073(10) 0.0531(6) Uani 1 1 d D . . . .
H1W1 H 1.485(4) 0.718(2) 1.1106(11) 0.064 Uiso 1 1 d D U . . .
H1W2 H 1.544(4) 0.7846(11) 1.1411(15) 0.064 Uiso 1 1 d D U . . .
Cl1 Cl 1.22041(7) 0.78698(4) 1.04366(2) 0.02425(12) Uani 1 1 d . . . . .
O11 O 1.0832(2) 0.74536(14) 1.06511(8) 0.0473(5) Uani 1 1 d . . . . .
O12 O 1.2745(3) 0.84732(12) 1.08428(8) 0.0449(5) Uani 1 1 d . . . . .
O13 O 1.3426(2) 0.72588(11) 1.03489(8) 0.0361(4) Uani 1 1 d . . . . .
O14 O 1.1822(2) 0.82692(11) 0.98999(7) 0.0328(4) Uani 1 1 d . . . . .
Cl2 Cl 0.70035(7) 0.56488(4) 0.67448(3) 0.03214(14) Uani 1 1 d . . . . .
O21A O 0.5267(8) 0.5665(6) 0.6723(4) 0.0262(18) Uiso 0.404(18) 1 d . . P A 1
O22A O 0.7346(16) 0.4817(6) 0.6961(7) 0.019(2) Uiso 0.404(18) 1 d . . P A 1
O23A O 0.7802(10) 0.6183(4) 0.7161(4) 0.033(2) Uiso 0.404(18) 1 d . . P A 1
O24A O 0.7737(10) 0.5683(8) 0.6200(3) 0.0260(19) Uiso 0.404(18) 1 d . . P A 1
O21B O 0.7940(9) 0.5985(8) 0.6291(4) 0.044(2) Uiso 0.330(13) 1 d . . P A 2
O22B O 0.7247(12) 0.6263(4) 0.7236(3) 0.034(2) Uiso 0.330(13) 1 d . . P A 2
O23B O 0.5335(9) 0.5771(6) 0.6566(4) 0.0269(19) Uiso 0.330(13) 1 d . . P A 2
O24B O 0.7174(14) 0.4844(7) 0.7065(5) 0.047(4) Uiso 0.330(13) 1 d . . P A 2
O21C O 0.7436(15) 0.5451(10) 0.6133(5) 0.042(3) Uiso 0.267(16) 1 d . . P A 3
O22C O 0.7725(13) 0.6304(8) 0.6972(8) 0.052(4) Uiso 0.267(16) 1 d . . P A 3
O23C O 0.7507(18) 0.4856(10) 0.6878(7) 0.040(6) Uiso 0.267(16) 1 d . . P A 3
O24C O 0.5442(11) 0.5860(8) 0.6747(6) 0.024(2) Uiso 0.267(16) 1 d . . P A 3


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Cd1 N1 2.3364(19) . ?
Cd1 N5 2.3390(18) . ?
Cd1 N6 2.3500(17) . ?
Cd1 N3 2.356(2) . ?
Cd1 N2 2.3888(18) . ?
Cd1 N4 2.4053(18) . ?
N3 C1 1.470(3) . ?
N3 C8 1.473(3) . ?
N2 C9 1.469(3) . ?
N2 C3 1.478(3) . ?
N2 C2 1.481(3) . ?
N1 C4 1.476(3) . ?
N1 C5 1.477(3) . ?
N4 C19 1.464(3) . ?
N4 C7 1.476(3) . ?
N4 C6 1.479(3) . ?
N5 C10 1.326(3) . ?
N5 C18 1.381(3) . ?
N6 C20 1.319(3) . ?
N6 C28 1.383(3) . ?
C1 C2 1.517(3) . ?
C3 C4 1.522(3) . ?
C5 C6 1.519(3) . ?
C7 C8 1.524(3) . ?
C9 C10 1.509(3) . ?
C10 C11 1.414(3) . ?
C11 C12 1.356(4) . ?
C12 C13 1.419(4) . ?
C13 C18 1.406(3) . ?
C13 C14 1.419(4) . ?
C14 C15 1.356(4) . ?
C15 C16 1.405(4) . ?
C16 C17 1.359(3) . ?
C17 C18 1.403(3) . ?
C19 C20 1.512(3) . ?
C20 C21 1.410(3) . ?
C21 C22 1.358(3) . ?
C22 C23 1.409(3) . ?
C23 C28 1.416(3) . ?
C23 C24 1.417(3) . ?
C24 C25 1.361(3) . ?
C25 C26 1.410(3) . ?
C26 C27 1.367(3) . ?
C27 C28 1.407(3) . ?
Cl1 O12 1.428(2) . ?
Cl1 O11 1.4341(19) . ?
Cl1 O14 1.4396(17) . ?
Cl1 O13 1.4420(18) . ?
Cl2 O22C 1.324(10) . ?
Cl2 O23C 1.377(15) . ?
Cl2 O24C 1.366(9) . ?
Cl2 O24A 1.416(6) . ?
Cl2 O23A 1.457(7) . ?
Cl2 O21A 1.473(7) . ?
Cl2 O22A 1.455(11) . ?
Cl2 O21B 1.431(8) . ?
Cl2 O23B 1.486(8) . ?
Cl2 O21C 1.508(11) . ?
Cl2 O22B 1.523(7) . ?
Cl2 O24B 1.498(12) . ?
O21C O23C 1.982(18) . ?

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 Cd1 N5 128.89(7) . . ?
N1 Cd1 N6 94.69(6) . . ?
N5 Cd1 N6 100.08(6) . . ?
N3 Cd1 N1 118.86(7) . . ?
N5 Cd1 N3 90.88(7) . . ?
N6 Cd1 N3 125.44(7) . . ?
N1 Cd1 N2 75.68(6) . . ?
N5 Cd1 N2 71.79(6) . . ?
N6 Cd1 N2 156.86(7) . . ?
N3 Cd1 N2 77.09(7) . . ?
N1 Cd1 N4 77.15(6) . . ?
N5 Cd1 N4 153.88(6) . . ?
N6 Cd1 N4 72.36(6) . . ?
N3 Cd1 N4 74.91(7) . . ?
N2 Cd1 N4 124.10(6) . . ?
C1 N3 C8 115.20(19) . . ?
C1 N3 Cd1 105.73(14) . . ?
C8 N3 Cd1 110.58(14) . . ?
C9 N2 C3 111.83(18) . . ?
C9 N2 C2 110.42(18) . . ?
C3 N2 C2 111.89(18) . . ?
C9 N2 Cd1 107.04(13) . . ?
C3 N2 Cd1 108.99(13) . . ?
C2 N2 Cd1 106.40(13) . . ?
C4 N1 C5 113.61(18) . . ?
C4 N1 Cd1 110.33(13) . . ?
C5 N1 Cd1 105.64(13) . . ?
C19 N4 C7 111.47(18) . . ?
C19 N4 C6 110.41(17) . . ?
C7 N4 C6 112.17(17) . . ?
C19 N4 Cd1 107.91(13) . . ?
C7 N4 Cd1 109.18(13) . . ?
C6 N4 Cd1 105.43(13) . . ?
C10 N5 C18 119.17(19) . . ?
C10 N5 Cd1 115.53(14) . . ?
C18 N5 Cd1 125.28(14) . . ?
C20 N6 C28 119.17(18) . . ?
C20 N6 Cd1 115.34(14) . . ?
C28 N6 Cd1 125.20(14) . . ?
N3 C1 C2 110.73(19) . . ?
N2 C2 C1 112.40(18) . . ?
N2 C3 C4 111.93(18) . . ?
N1 C4 C3 111.63(18) . . ?
N1 C5 C6 109.51(18) . . ?
N4 C6 C5 112.13(18) . . ?
N4 C7 C8 111.70(18) . . ?
N3 C8 C7 111.20(19) . . ?
N2 C9 C10 112.29(19) . . ?
N5 C10 C11 122.3(2) . . ?
N5 C10 C9 118.35(19) . . ?
C11 C10 C9 119.3(2) . . ?
C12 C11 C10 119.3(2) . . ?
C11 C12 C13 120.1(2) . . ?
C18 C13 C12 117.8(2) . . ?
C18 C13 C14 118.9(2) . . ?
C12 C13 C14 123.4(2) . . ?
C15 C14 C13 120.4(3) . . ?
C14 C15 C16 120.5(3) . . ?
C17 C16 C15 120.1(2) . . ?
C16 C17 C18 120.9(2) . . ?
N5 C18 C17 119.5(2) . . ?
N5 C18 C13 121.3(2) . . ?
C17 C18 C13 119.2(2) . . ?
N4 C19 C20 113.68(19) . . ?
N6 C20 C21 122.2(2) . . ?
N6 C20 C19 119.61(19) . . ?
C21 C20 C19 118.1(2) . . ?
C22 C21 C20 119.8(2) . . ?
C21 C22 C23 119.8(2) . . ?
C22 C23 C28 117.7(2) . . ?
C22 C23 C24 123.3(2) . . ?
C28 C23 C24 119.0(2) . . ?
C25 C24 C23 120.6(2) . . ?
C24 C25 C26 120.1(2) . . ?
C27 C26 C25 120.7(2) . . ?
C26 C27 C28 120.3(2) . . ?
N6 C28 C27 119.58(19) . . ?
N6 C28 C23 121.2(2) . . ?
C27 C28 C23 119.2(2) . . ?
O12 Cl1 O11 110.09(13) . . ?
O12 Cl1 O14 110.06(12) . . ?
O11 Cl1 O14 109.33(11) . . ?
O12 Cl1 O13 109.07(12) . . ?
O11 Cl1 O13 108.53(12) . . ?
O14 Cl1 O13 109.74(11) . . ?
O22C Cl2 O23C 120.1(9) . . ?
O22C Cl2 O24C 104.3(8) . . ?
O23C Cl2 O24C 121.8(10) . . ?
O24A Cl2 O23A 111.5(5) . . ?
O24A Cl2 O21A 114.4(5) . . ?
O23A Cl2 O21A 118.2(5) . . ?
O24A Cl2 O22A 104.9(9) . . ?
O23A Cl2 O22A 102.7(6) . . ?
O21A Cl2 O22A 103.0(7) . . ?
O21B Cl2 O23B 105.9(4) . . ?
O22C Cl2 O21C 115.5(6) . . ?
O23C Cl2 O21C 86.6(9) . . ?
O24C Cl2 O21C 107.3(6) . . ?
O21B Cl2 O22B 103.7(5) . . ?
O23B Cl2 O22B 104.5(5) . . ?
O21B Cl2 O24B 129.8(7) . . ?
O23B Cl2 O24B 110.0(6) . . ?
O22B Cl2 O24B 99.9(5) . . ?
Cl2 O21C O23C 43.9(5) . . ?
Cl2 O23C O21C 49.4(7) . . ?

_refine_diff_density_max         0.521
_refine_diff_density_min         -0.559
_refine_diff_density_rms         0.071



