# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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. 
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data_e18adb4
_database_code_depnum_ccdc_archive 'CCDC 2097428'
loop_
_audit_author_name
_audit_author_address
'Mary Mahon'
;University of Bath
United Kingdom
;
_audit_update_record             
;
2021-07-19 deposited with the CCDC.	2021-12-20 downloaded from the CCDC.
;
_audit_creation_date             2019-01-11
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelxl_version_number           2014-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C20 H18 Cd2 N2 O14, H2 O'
_chemical_formula_sum            'C20 H20 Cd2 N2 O15'
_chemical_formula_weight         753.18
_chemical_melting_point          ?
_chemical_oxdiff_usercomment     'Light Brown Tablet'
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'
Cd Cd -0.8075 1.2024 '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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 1 2/a 1'
_space_group_name_Hall           '-I 2ya'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'

_cell_length_a                   13.7701(4)
_cell_length_b                   11.5100(3)
_cell_length_c                   29.1745(7)
_cell_angle_alpha                90
_cell_angle_beta                 90.088(2)
_cell_angle_gamma                90
_cell_volume                     4624.0(2)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    14938
_cell_measurement_temperature    150.0(3)
_cell_measurement_theta_max      30.1010
_cell_measurement_theta_min      3.9110
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.925
_exptl_absorpt_correction_T_max  0.994
_exptl_absorpt_correction_T_min  0.974
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light brown'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    2.164
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2960
_exptl_crystal_size_max          0.291
_exptl_crystal_size_mid          0.231
_exptl_crystal_size_min          0.063
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0246
_diffrn_reflns_av_unetI/netI     0.0247
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.887
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            21531
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.887
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.343
_diffrn_reflns_theta_min         3.517
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.0(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0734
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.887
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5621
_reflns_number_total             6180
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         1.655
_refine_diff_density_min         -3.605
_refine_diff_density_rms         0.115
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     390
_refine_ls_number_reflns         6180
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0321
_refine_ls_restrained_S_all      1.074
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0116P)²+35.2439P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0638
_refine_ls_wR_factor_ref         0.0659
_refine_special_details          
;
The asymmetric unit comprises 2 cadmium centres, 2 doubly-deprotonated 
5-CMAI ligands, 2 water ligands and 1 lattice water. The largest residual peak 
and hole in the difference electron density map are in the region of Cd2 and 
the ADP for this atom is elongated. Attempts were made to model disorder for 
Cd2, but these were ultimately abandoned as a similar (obligatory) disorder 
could not be modelled for the atoms ligated to each disordered component of 
the metal. As such, the model lost chemical integrity. 
2-dimensional polymeric sheets dominate the gross structure and these 
propagate in the ab plane. 
The water hydrogens, along with those bound to N1, N2, O6 and O12, were 
located and refined at a distance of 0.98Å from the relevant parent atom. 
Additional distance restraints (2.75 Å for Cd2?H14a and Cd2?H14b, and 
1.5Å for  H14a?H14b) were included, to assist convergence. The least 
reliable hydrogen positions pertain to H14a and H14b. All of the 'located' 
hydrogens are implicated in hydrogen-bonding, which links the covalently 
bonded sheets, which stack along c, to form a 3-D network in the 
gross structure. 

;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H,H) groups
2. Restrained distances
 O6-H6 = O12-H12
 0.98 with sigma of 0.005
 N1-H1 = N2-H2
 0.98 with sigma of 0.005
 O15-H15A = O15-H15B
 0.98 with sigma of 0.005
 O14-H14B
 0.98 with sigma of 0.005
 H14B-H14A
 1.55 with sigma of 0.005
 O14-H14A
 0.98 with sigma of 0.005
 H14A-Cd2 = H14B-Cd2
 2.75 with sigma of 0.02
 O13-H13A = O13-H13B
 0.98 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Uanis(Cd2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C12(H12A,H12B)
4.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C7(H7), C10(H10), C14(H14), C17(H17), C20(H20)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
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 0.74587(2) 0.63625(2) 0.56339(2) 0.01141(5) Uani 1 1 d . . . . .
O1 O 0.68210(17) 0.42539(18) 0.58131(8) 0.0221(5) Uani 1 1 d . . . . .
O2 O 0.83218(16) 0.48453(18) 0.59175(7) 0.0191(4) Uani 1 1 d . . . . .
O3 O 0.76611(16) -0.16000(17) 0.57335(7) 0.0158(4) Uani 1 1 d . . . . .
O4 O 0.77767(16) -0.27694(17) 0.63271(6) 0.0152(4) Uani 1 1 d . . . . .
O5 O 0.7390(2) 0.0577(2) 0.80253(8) 0.0325(6) Uani 1 1 d . . . . .
O6 O 0.7300(2) -0.1293(2) 0.78467(8) 0.0340(6) Uani 1 1 d D . . . .
H6 H 0.724(4) -0.148(5) 0.8173(5) 0.079(19) Uiso 1 1 d D . . . .
O7 O 0.65443(16) 0.6387(2) 0.49934(7) 0.0218(5) Uani 1 1 d . . . . .
O8 O 0.5133(2) 0.6488(3) 0.46466(9) 0.0411(7) Uani 1 1 d . . . . .
O9 O 0.52332(16) 1.08681(18) 0.58216(7) 0.0180(4) Uani 1 1 d . . . . .
O10 O 0.49804(16) 1.14172(17) 0.65311(7) 0.0163(4) Uani 1 1 d . . . . .
O11 O 0.4749(2) 0.8417(2) 0.77469(8) 0.0316(6) Uani 1 1 d . . . . .
O12 O 0.52285(19) 0.66127(19) 0.75910(7) 0.0253(5) Uani 1 1 d D . . . .
H12 H 0.513(4) 0.653(5) 0.7922(4) 0.076(18) Uiso 1 1 d D . . . .
O13 O 0.49734(18) 0.4160(2) 0.63637(8) 0.0238(5) Uani 1 1 d D . . . .
O14 O 0.6630(2) 0.1944(3) 0.52291(10) 0.0405(7) Uani 1 1 d D . . . .
H14A H 0.633(2) 0.252(2) 0.5027(6) 0.049 Uiso 1 1 d DR . . . .
H14B H 0.6231(19) 0.1248(16) 0.5198(9) 0.049 Uiso 1 1 d DR . . . .
N1 N 0.70857(17) 0.24368(19) 0.64105(8) 0.0114(4) Uani 1 1 d D . . . .
H1 H 0.690(3) 0.292(3) 0.6673(8) 0.027(10) Uiso 1 1 d D . . . .
N2 N 0.57199(19) 0.6505(2) 0.58673(8) 0.0154(5) Uani 1 1 d D . . . .
H2 H 0.569(3) 0.5751(15) 0.6021(11) 0.021(9) Uiso 1 1 d D . . . .
C1 C 0.7669(2) 0.4092(2) 0.59554(9) 0.0137(5) Uani 1 1 d . . . . .
C2 C 0.7933(2) 0.2940(2) 0.61739(10) 0.0150(5) Uani 1 1 d . . . . .
H2A H 0.8157 0.2407 0.5940 0.018 Uiso 1 1 calc R . . . .
H2B H 0.8456 0.3055 0.6392 0.018 Uiso 1 1 calc R . . . .
C3 C 0.72764(19) 0.1297(2) 0.65919(9) 0.0116(5) Uani 1 1 d . . . . .
C4 C 0.74515(19) 0.0367(2) 0.62967(9) 0.0113(5) Uani 1 1 d . . . . .
H4 H 0.7465 0.0487 0.5981 0.014 Uiso 1 1 calc R . . . .
C5 C 0.76051(19) -0.0737(2) 0.64736(9) 0.0108(5) Uani 1 1 d . . . . .
C6 C 0.7705(2) -0.1752(2) 0.61598(9) 0.0117(5) Uani 1 1 d . . . . .
C7 C 0.7582(2) -0.0915(2) 0.69464(9) 0.0127(5) Uani 1 1 d . . . . .
H7 H 0.7685 -0.1655 0.7065 0.015 Uiso 1 1 calc R . . . .
C8 C 0.7408(2) 0.0008(2) 0.72392(9) 0.0130(5) Uani 1 1 d . . . . .
C9 C 0.7370(2) -0.0188(3) 0.77456(10) 0.0173(6) Uani 1 1 d . . . . .
C10 C 0.7254(2) 0.1118(2) 0.70643(9) 0.0129(5) Uani 1 1 d . . . . .
H10 H 0.7138 0.1737 0.7262 0.015 Uiso 1 1 calc R . . . .
C11 C 0.5637(2) 0.6471(2) 0.49964(10) 0.0161(6) Uani 1 1 d . . . . .
C12 C 0.5106(2) 0.6499(3) 0.54478(10) 0.0192(6) Uani 1 1 d . . . . .
H12A H 0.4698 0.7186 0.5453 0.023 Uiso 1 1 calc R . . . .
H12B H 0.4681 0.5828 0.5462 0.023 Uiso 1 1 calc R . . . .
C13 C 0.5479(2) 0.7381(2) 0.61974(9) 0.0126(5) Uani 1 1 d . . . . .
C14 C 0.5365(2) 0.8527(2) 0.60611(9) 0.0128(5) Uani 1 1 d . . . . .
H14 H 0.5456 0.8729 0.5755 0.015 Uiso 1 1 calc R . . . .
C15 C 0.5115(2) 0.9379(2) 0.63808(9) 0.0112(5) Uani 1 1 d . . . . .
C16 C 0.50864(19) 1.0625(2) 0.62388(9) 0.0119(5) Uani 1 1 d . . . . .
C17 C 0.4983(2) 0.9079(2) 0.68377(9) 0.0136(5) Uani 1 1 d . . . . .
H17 H 0.4797 0.9639 0.7050 0.016 Uiso 1 1 calc R . . . .
C18 C 0.5130(2) 0.7940(2) 0.69757(9) 0.0134(5) Uani 1 1 d . . . . .
C19 C 0.5022(2) 0.7682(3) 0.74747(10) 0.0176(6) Uani 1 1 d . . . . .
C20 C 0.5381(2) 0.7086(2) 0.66584(9) 0.0137(5) Uani 1 1 d . . . . .
H20 H 0.5483 0.6325 0.6754 0.016 Uiso 1 1 calc R . . . .
Cd2 Cd 0.57197(2) 0.27393(2) 0.59213(2) 0.02749(7) Uani 1 1 d D U . . .
O15 O 0.6112(3) -0.0239(4) 0.48765(13) 0.0701(13) Uani 1 1 d D . . . .
H15A H 0.555(3) -0.029(7) 0.4672(19) 0.12(3) Uiso 1 1 d D . . . .
H15B H 0.670(3) -0.064(6) 0.478(2) 0.13(3) Uiso 1 1 d D . . . .
H13A H 0.4330(15) 0.449(4) 0.6306(16) 0.050(14) Uiso 1 1 d D . . . .
H13B H 0.489(5) 0.391(5) 0.6682(7) 0.09(2) Uiso 1 1 d 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
Cd1 O1 2.634(2) . ?
Cd1 O2 2.268(2) . ?
Cd1 O3 2.379(2) 1_565 ?
Cd1 O4 2.2973(19) 1_565 ?
Cd1 O7 2.252(2) . ?
Cd1 O7 2.290(2) 2_656 ?
Cd1 N2 2.496(3) . ?
O1 C1 1.253(4) . ?
O1 Cd2 2.332(2) . ?
O2 C1 1.253(4) . ?
O3 Cd1 2.379(2) 1_545 ?
O3 C6 1.257(3) . ?
O4 Cd1 2.2971(19) 1_545 ?
O4 C6 1.272(3) . ?
O5 C9 1.201(4) . ?
O6 H6 0.979(5) . ?
O6 C9 1.309(4) . ?
O7 Cd1 2.290(2) 2_656 ?
O7 C11 1.254(4) . ?
O8 C11 1.233(4) . ?
O8 Cd2 2.216(2) 5_666 ?
O9 C16 1.265(3) . ?
O9 Cd2 2.274(2) 1_565 ?
O10 C16 1.257(3) . ?
O10 Cd2 2.554(2) 1_565 ?
O11 C19 1.219(4) . ?
O12 H12 0.979(5) . ?
O12 C19 1.308(4) . ?
O13 Cd2 2.324(3) . ?
O13 H13A 0.978(5) . ?
O13 H13B 0.978(5) . ?
O14 H14A 0.978(5) . ?
O14 H14B 0.976(5) . ?
O14 Cd2 2.549(3) . ?
N1 H1 0.979(5) . ?
N1 C2 1.475(4) . ?
N1 C3 1.439(3) . ?
N1 Cd2 2.385(2) . ?
N2 H2 0.979(5) . ?
N2 C12 1.487(4) . ?
N2 C13 1.433(3) . ?
C1 C2 1.515(4) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.395(4) . ?
C3 C10 1.394(4) . ?
C4 H4 0.9300 . ?
C4 C5 1.387(4) . ?
C5 C6 1.492(4) . ?
C5 C7 1.395(4) . ?
C6 Cd1 2.679(3) 1_545 ?
C7 H7 0.9300 . ?
C7 C8 1.385(4) . ?
C8 C9 1.496(4) . ?
C8 C10 1.392(4) . ?
C10 H10 0.9300 . ?
C11 C12 1.507(4) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C14 1.387(4) . ?
C13 C20 1.394(4) . ?
C14 H14 0.9300 . ?
C14 C15 1.397(4) . ?
C15 C16 1.493(4) . ?
C15 C17 1.389(4) . ?
C16 Cd2 2.746(3) 1_565 ?
C17 H17 0.9300 . ?
C17 C18 1.386(4) . ?
C18 C19 1.493(4) . ?
C18 C20 1.394(4) . ?
C20 H20 0.9300 . ?
Cd2 O8 2.216(2) 5_666 ?
Cd2 O9 2.274(2) 1_545 ?
Cd2 O10 2.554(2) 1_545 ?
Cd2 C16 2.746(3) 1_545 ?
O15 H15A 0.979(5) . ?
O15 H15B 0.979(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
O2 Cd1 O1 52.61(7) . . ?
O2 Cd1 O3 130.78(8) . 1_565 ?
O2 Cd1 O4 85.10(8) . 1_565 ?
O2 Cd1 O7 89.23(8) . 2_656 ?
O2 Cd1 N2 116.98(8) . . ?
O3 Cd1 O1 157.37(7) 1_565 . ?
O3 Cd1 N2 90.80(8) 1_565 . ?
O4 Cd1 O1 106.81(7) 1_565 . ?
O4 Cd1 O3 56.06(7) 1_565 1_565 ?
O4 Cd1 N2 84.99(8) 1_565 . ?
O7 Cd1 O1 89.42(8) . . ?
O7 Cd1 O1 111.74(8) 2_656 . ?
O7 Cd1 O2 127.18(8) . . ?
O7 Cd1 O3 90.88(8) 2_656 1_565 ?
O7 Cd1 O3 98.88(8) . 1_565 ?
O7 Cd1 O4 146.17(8) . 1_565 ?
O7 Cd1 O4 125.78(8) 2_656 1_565 ?
O7 Cd1 O7 70.84(9) . 2_656 ?
O7 Cd1 N2 71.95(8) . . ?
O7 Cd1 N2 142.56(8) 2_656 . ?
N2 Cd1 O1 71.72(8) . . ?
C1 O1 Cd1 83.77(17) . . ?
C1 O1 Cd2 116.77(18) . . ?
Cd2 O1 Cd1 158.86(10) . . ?
C1 O2 Cd1 100.91(18) . . ?
C6 O3 Cd1 89.35(16) . 1_545 ?
C6 O4 Cd1 92.75(16) . 1_545 ?
C9 O6 H6 116(4) . . ?
Cd1 O7 Cd1 109.14(9) . 2_656 ?
C11 O7 Cd1 123.46(18) . . ?
C11 O7 Cd1 127.27(18) . 2_656 ?
C11 O8 Cd2 157.2(3) . 5_666 ?
C16 O9 Cd2 97.68(17) . 1_565 ?
C16 O10 Cd2 84.98(16) . 1_565 ?
C19 O12 H12 109(3) . . ?
Cd2 O13 H13A 125(3) . . ?
Cd2 O13 H13B 112(4) . . ?
H13A O13 H13B 100(5) . . ?
H14A O14 H14B 104.9(7) . . ?
Cd2 O14 H14A 91.5(12) . . ?
Cd2 O14 H14B 95.2(12) . . ?
C2 N1 H1 111(2) . . ?
C2 N1 Cd2 106.63(16) . . ?
C3 N1 H1 106(2) . . ?
C3 N1 C2 112.7(2) . . ?
C3 N1 Cd2 119.77(16) . . ?
Cd2 N1 H1 100(2) . . ?
Cd1 N2 H2 96(2) . . ?
C12 N2 Cd1 108.64(17) . . ?
C12 N2 H2 110(2) . . ?
C13 N2 Cd1 116.93(18) . . ?
C13 N2 H2 108(2) . . ?
C13 N2 C12 115.1(2) . . ?
O1 C1 O2 122.4(3) . . ?
O1 C1 C2 119.4(3) . . ?
O2 C1 C2 118.1(3) . . ?
N1 C2 C1 110.6(2) . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 108.1 . . ?
C4 C3 N1 120.3(2) . . ?
C10 C3 N1 119.6(2) . . ?
C10 C3 C4 120.1(2) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 C3 119.9(2) . . ?
C5 C4 H4 120.0 . . ?
C4 C5 C6 120.2(2) . . ?
C4 C5 C7 120.0(2) . . ?
C7 C5 C6 119.6(2) . . ?
O3 C6 Cd1 62.65(14) . 1_545 ?
O3 C6 O4 120.8(2) . . ?
O3 C6 C5 119.6(2) . . ?
O4 C6 Cd1 58.94(13) . 1_545 ?
O4 C6 C5 119.5(2) . . ?
C5 C6 Cd1 167.12(19) . 1_545 ?
C5 C7 H7 120.0 . . ?
C8 C7 C5 120.1(2) . . ?
C8 C7 H7 120.0 . . ?
C7 C8 C9 120.0(2) . . ?
C7 C8 C10 120.3(2) . . ?
C10 C8 C9 119.7(2) . . ?
O5 C9 O6 124.1(3) . . ?
O5 C9 C8 124.0(3) . . ?
O6 C9 C8 111.8(2) . . ?
C3 C10 H10 120.2 . . ?
C8 C10 C3 119.6(2) . . ?
C8 C10 H10 120.2 . . ?
O7 C11 C12 119.5(2) . . ?
O8 C11 O7 123.7(3) . . ?
O8 C11 C12 116.7(3) . . ?
N2 C12 C11 116.3(2) . . ?
N2 C12 H12A 108.2 . . ?
N2 C12 H12B 108.2 . . ?
C11 C12 H12A 108.2 . . ?
C11 C12 H12B 108.2 . . ?
H12A C12 H12B 107.4 . . ?
C14 C13 N2 120.2(2) . . ?
C14 C13 C20 119.8(2) . . ?
C20 C13 N2 120.0(2) . . ?
C13 C14 H14 119.9 . . ?
C13 C14 C15 120.3(2) . . ?
C15 C14 H14 119.9 . . ?
C14 C15 C16 119.7(2) . . ?
C17 C15 C14 119.9(2) . . ?
C17 C15 C16 120.1(2) . . ?
O9 C16 C15 118.3(2) . . ?
O9 C16 Cd2 55.15(14) . 1_565 ?
O10 C16 O9 120.8(3) . . ?
O10 C16 C15 120.7(2) . . ?
O10 C16 Cd2 67.89(15) . 1_565 ?
C15 C16 Cd2 159.44(19) . 1_565 ?
C15 C17 H17 120.2 . . ?
C18 C17 C15 119.7(3) . . ?
C18 C17 H17 120.2 . . ?
C17 C18 C19 117.2(2) . . ?
C17 C18 C20 120.7(3) . . ?
C20 C18 C19 122.2(3) . . ?
O11 C19 O12 123.4(3) . . ?
O11 C19 C18 121.9(3) . . ?
O12 C19 C18 114.7(3) . . ?
C13 C20 C18 119.6(3) . . ?
C13 C20 H20 120.2 . . ?
C18 C20 H20 120.2 . . ?
O1 Cd2 O10 143.09(7) . 1_545 ?
O1 Cd2 O14 80.81(10) . . ?
O1 Cd2 N1 71.20(8) . . ?
O1 Cd2 C16 156.17(8) . 1_545 ?
O8 Cd2 O1 86.71(9) 5_666 . ?
O8 Cd2 O9 97.41(9) 5_666 1_545 ?
O8 Cd2 O10 123.28(10) 5_666 1_545 ?
O8 Cd2 O13 84.17(10) 5_666 . ?
O8 Cd2 O14 79.18(11) 5_666 . ?
O8 Cd2 N1 157.32(10) 5_666 . ?
O8 Cd2 C16 116.09(9) 5_666 1_545 ?
O9 Cd2 O1 151.89(8) 1_545 . ?
O9 Cd2 O10 53.64(7) 1_545 1_545 ?
O9 Cd2 O13 127.38(8) 1_545 . ?
O9 Cd2 O14 72.78(9) 1_545 . ?
O9 Cd2 N1 99.80(8) 1_545 . ?
O9 Cd2 C16 27.17(7) 1_545 1_545 ?
O10 Cd2 C16 27.12(7) 1_545 1_545 ?
O13 Cd2 O1 80.64(8) . . ?
O13 Cd2 O10 81.68(7) . 1_545 ?
O13 Cd2 O14 155.67(9) . . ?
O13 Cd2 N1 96.86(8) . . ?
O13 Cd2 C16 107.18(8) . 1_545 ?
O14 Cd2 O10 122.36(8) . 1_545 ?
O14 Cd2 C16 96.09(9) . 1_545 ?
N1 Cd2 O10 79.11(7) . 1_545 ?
N1 Cd2 O14 91.91(9) . . ?
N1 Cd2 C16 85.37(8) . 1_545 ?
H15A O15 H15B 117(6) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O6 H6 O4 0.979(5) 1.696(19) 2.643(3) 162(5) 7_646
O12 H12 O10 0.979(5) 1.609(7) 2.587(3) 177(6) 4_546
O14 H14A O8 0.978(5) 2.50(2) 3.047(4) 114.9(15) 5_666
O14 H14B O9 0.976(5) 2.32(2) 2.870(4) 114.6(15) 1_545
O14 H14B O15 0.976(5) 1.959(13) 2.807(5) 143.9(18) .
N1 H1 O5 0.979(5) 2.18(3) 2.907(3) 130(3) 7_656
N2 H2 O1 0.979(5) 2.40(3) 3.007(3) 119(3) .
O15 H15A O9 0.979(5) 1.92(3) 2.845(4) 157(6) 5_666
O15 H15A O15 0.979(5) 2.71(7) 3.195(7) 111(5) 5_656
O15 H15B O3 0.979(5) 2.05(4) 2.913(4) 145(6) 2_656
O13 H13A O2 0.978(5) 1.95(2) 2.858(3) 154(4) 6_565
O13 H13B O11 0.978(5) 1.83(3) 2.758(3) 158(6) 4_546


_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_s18adb31
_database_code_depnum_ccdc_archive 'CCDC 2097431'
loop_
_audit_author_name
_audit_author_address
'Mary Mahon'
;University of Bath
United Kingdom
;
_audit_update_record             
;
2021-07-22 deposited with the CCDC.	2021-12-20 downloaded from the CCDC.
;
_audit_creation_date             2018-10-25
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelxl_version_number           2014-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C20 H12 Cd3 N2 O12'
_chemical_formula_sum            'C20 H12 Cd3 N2 O12'
_chemical_formula_weight         809.52
_chemical_melting_point          ?
_chemical_oxdiff_usercomment     'Colourless Plate'
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'
Cd Cd 0.1185 4.6533 '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'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.0862(15)
_cell_length_b                   8.1863(13)
_cell_length_c                   8.4893(11)
_cell_angle_alpha                72.651(13)
_cell_angle_beta                 81.681(13)
_cell_angle_gamma                65.767(17)
_cell_volume                     488.97(15)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    1188
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      71.6780
_cell_measurement_theta_min      5.4630
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    26.648
_exptl_absorpt_correction_T_max  0.54577
_exptl_absorpt_correction_T_min  0.50765
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.749
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             386
_exptl_crystal_size_max          0.064
_exptl_crystal_size_mid          0.033
_exptl_crystal_size_min          0.015
_exptl_crystal_size_rad          0.044
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_av_unetI/netI     0.0537
_diffrn_reflns_Laue_measured_fraction_full 0.915
_diffrn_reflns_Laue_measured_fraction_max 0.914
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            2549
_diffrn_reflns_point_group_measured_fraction_full 0.915
_diffrn_reflns_point_group_measured_fraction_max 0.914
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.176
_diffrn_reflns_theta_min         6.003
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1150
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.915
_diffrn_measured_fraction_theta_max 0.914
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1356
_reflns_number_total             1632
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         1.883
_refine_diff_density_min         -1.312
_refine_diff_density_rms         0.218
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         1632
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0488
_refine_ls_restrained_S_all      1.045
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0790P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1187
_refine_ls_wR_factor_ref         0.1273
_refine_special_details          
;
The asymmetric unit contains one full cadmium centre (Cd1), one 
half-occupancy cadmium centre (Cd2, residing on a special position) 
and one full 5-((carboxylatomethyl)amino)-isophthalate ligand 
(5-CMAI), giving an empirical formula of [Cd3(5-CMAI)2]. Cd1 
was found to be 7 coordinate and is ligated by 4 distinct 
5-CMAI anions, through 6 oxygen and 1 nitrogen atoms.  Cd2 
resides on a centre of inversion, is 6 coordinate, and 
exhibits distorted octahedral in geometry with O-Cd-O 
angles ranging from 72.6(2) to 107.4(2)o. Overall, the 
structure is a dense 3-D network, with a consolidating 
hydrogen-bond between the amine hydrogen in the ASU and 
O1 in a proximate motif. 
The diffraction pattern was not of premium quality. The 
data were integrated initially to take account of twinning, 
but the level of peak overlap rendered it difficult to 
de-convolute the component intensity data . Ultimately, 
the raw data were integrated by increasing the integration 
mask (1.5 x default mask size) and profile size altering 
with incident angle. Essentially, this treated split peaks 
as arising from a slightly cracked crystal rather than a 
well-defined twin. The latter approach gave the most 
satisfactory residuals and Rint. A side by side comparison 
of the outputs from both data treatments showed that the 
optimal one chosen did not negatively impact on the esds 
associated with the bond/angle metrics. The completeness 
of the data is less than ideal, but the structure is unambiguous.

;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 N1-H1
 0.98 with sigma of 0.005
3.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C10(H10), C7(H7)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
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
Cd2 Cd 0.5000 1.0000 0.0000 0.0272(3) Uani 1 2 d S T P . .
Cd1 Cd 0.88744(9) -0.00936(8) 0.20601(8) 0.0256(2) Uani 1 1 d . . . . .
O4 O 0.0946(9) 0.7763(8) 0.0772(8) 0.0254(14) Uani 1 1 d . . . . .
O3 O 0.3409(9) 0.8222(8) -0.0223(7) 0.0259(14) Uani 1 1 d . . . . .
O1 O 1.1592(9) 0.0085(9) 0.2400(8) 0.0312(15) Uani 1 1 d . . . . .
O5 O 0.1404(10) 0.2211(10) 0.5635(8) 0.0353(17) Uani 1 1 d . . . . .
N1 N 0.8463(11) 0.2463(11) 0.3168(9) 0.0263(17) Uani 1 1 d D . . . .
O2 O 1.2638(10) 0.2227(10) 0.0852(9) 0.0362(17) Uani 1 1 d . . . . .
O6 O 0.3585(12) 0.1379(10) 0.7370(9) 0.044(2) Uani 1 1 d . . . . .
C8 C 0.3780(13) 0.3335(13) 0.4678(11) 0.0240(19) Uani 1 1 d . . . . .
C9 C 0.2884(15) 0.2267(13) 0.5975(12) 0.031(2) Uani 1 1 d . . . . .
C4 C 0.5590(13) 0.5004(12) 0.2087(11) 0.0244(19) Uani 1 1 d . . . . .
H4 H 0.6186 0.5569 0.1221 0.029 Uiso 1 1 calc R . . . .
C3 C 0.6560(13) 0.3450(13) 0.3290(11) 0.028(2) Uani 1 1 d . . . . .
C2 C 0.9689(13) 0.3299(13) 0.2114(12) 0.028(2) Uani 1 1 d . . . . .
H2A H 0.9955 0.4039 0.2668 0.034 Uiso 1 1 calc R . . . .
H2B H 0.9111 0.4104 0.1083 0.034 Uiso 1 1 calc R . . . .
C6 C 0.2611(14) 0.7340(12) 0.0862(10) 0.025(2) Uani 1 1 d . . . . .
C5 C 0.3700(13) 0.5706(12) 0.2203(10) 0.0231(19) Uani 1 1 d . . . . .
C10 C 0.5657(14) 0.2637(12) 0.4607(11) 0.028(2) Uani 1 1 d . . . . .
H10 H 0.6316 0.1626 0.5437 0.034 Uiso 1 1 calc R . . . .
C7 C 0.2767(14) 0.4869(13) 0.3463(12) 0.029(2) Uani 1 1 d . . . . .
H7 H 0.1506 0.5319 0.3492 0.035 Uiso 1 1 calc R . . . .
C1 C 1.1441(13) 0.1748(13) 0.1773(11) 0.026(2) Uani 1 1 d . . . . .
H1 H 0.883(16) 0.173(14) 0.430(5) 0.05(4) Uiso 1 1 d 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
Cd2 O3 2.363(6) . ?
Cd2 O3 2.363(6) 2_675 ?
Cd2 O2 2.241(7) 2_765 ?
Cd2 O2 2.241(7) 1_465 ?
Cd2 O6 2.396(7) 2_666 ?
Cd2 O6 2.396(7) 1_564 ?
Cd1 O4 2.614(6) 2_665 ?
Cd1 O4 2.298(6) 1_645 ?
Cd1 O3 2.297(6) 2_665 ?
Cd1 O1 2.325(7) . ?
Cd1 O5 2.248(6) 2_656 ?
Cd1 N1 2.426(8) . ?
Cd1 O6 2.537(8) 2_656 ?
Cd1 C9 2.755(10) 2_656 ?
O4 Cd1 2.614(6) 2_665 ?
O4 Cd1 2.298(6) 1_465 ?
O4 C6 1.253(12) . ?
O3 Cd1 2.297(6) 2_665 ?
O3 C6 1.265(11) . ?
O1 C1 1.265(11) . ?
O5 Cd1 2.248(6) 2_656 ?
O5 C9 1.293(13) . ?
N1 C3 1.419(12) . ?
N1 C2 1.479(12) . ?
O2 Cd2 2.241(7) 1_645 ?
O2 C1 1.270(11) . ?
O6 Cd2 2.396(7) 1_546 ?
O6 Cd1 2.537(8) 2_656 ?
O6 C9 1.263(11) . ?
C8 C9 1.488(13) . ?
C8 C10 1.384(14) . ?
C8 C7 1.393(13) . ?
C9 Cd1 2.755(10) 2_656 ?
C4 C3 1.383(12) . ?
C4 C5 1.395(13) . ?
C3 C10 1.395(13) . ?
C2 C1 1.526(13) . ?
C6 C5 1.509(11) . ?
C5 C7 1.392(13) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Cd2 O3 180.0 2_675 . ?
O3 Cd2 O6 72.6(2) . 1_564 ?
O3 Cd2 O6 72.6(2) 2_675 2_666 ?
O3 Cd2 O6 107.4(2) 2_675 1_564 ?
O3 Cd2 O6 107.4(2) . 2_666 ?
O2 Cd2 O3 82.9(3) 1_465 2_675 ?
O2 Cd2 O3 97.1(3) 1_465 . ?
O2 Cd2 O3 82.9(3) 2_765 . ?
O2 Cd2 O3 97.1(3) 2_765 2_675 ?
O2 Cd2 O2 180.0 2_765 1_465 ?
O2 Cd2 O6 94.4(3) 2_765 1_564 ?
O2 Cd2 O6 85.6(3) 2_765 2_666 ?
O2 Cd2 O6 94.4(3) 1_465 2_666 ?
O2 Cd2 O6 85.6(3) 1_465 1_564 ?
O6 Cd2 O6 180.0 2_666 1_564 ?
O4 Cd1 O4 82.7(2) 1_645 2_665 ?
O4 Cd1 O1 77.6(2) 1_645 . ?
O4 Cd1 N1 143.3(3) 1_645 . ?
O4 Cd1 O6 97.7(3) 1_645 2_656 ?
O4 Cd1 C9 147.5(3) 2_665 2_656 ?
O4 Cd1 C9 98.6(3) 1_645 2_656 ?
O3 Cd1 O4 52.3(2) 2_665 2_665 ?
O3 Cd1 O4 106.1(2) 2_665 1_645 ?
O3 Cd1 O1 131.3(2) 2_665 . ?
O3 Cd1 N1 91.7(2) 2_665 . ?
O3 Cd1 O6 71.1(2) 2_665 2_656 ?
O3 Cd1 C9 97.1(3) 2_665 2_656 ?
O1 Cd1 O4 81.2(2) . 2_665 ?
O1 Cd1 N1 66.8(3) . . ?
O1 Cd1 O6 157.6(2) . 2_656 ?
O1 Cd1 C9 131.0(3) . 2_656 ?
O5 Cd1 O4 174.4(2) 2_656 2_665 ?
O5 Cd1 O4 95.0(2) 2_656 1_645 ?
O5 Cd1 O3 124.1(3) 2_656 2_665 ?
O5 Cd1 O1 103.4(3) 2_656 . ?
O5 Cd1 N1 101.2(3) 2_656 . ?
O5 Cd1 O6 54.8(2) 2_656 2_656 ?
O5 Cd1 C9 27.7(3) 2_656 2_656 ?
N1 Cd1 O4 83.5(2) . 2_665 ?
N1 Cd1 O6 118.5(3) . 2_656 ?
N1 Cd1 C9 111.0(3) . 2_656 ?
O6 Cd1 O4 120.3(2) 2_656 2_665 ?
O6 Cd1 C9 27.2(3) 2_656 2_656 ?
Cd1 O4 Cd1 97.3(2) 1_465 2_665 ?
C6 O4 Cd1 120.2(6) . 1_465 ?
C6 O4 Cd1 86.3(5) . 2_665 ?
Cd1 O3 Cd2 107.9(2) 2_665 . ?
C6 O3 Cd2 131.0(6) . . ?
C6 O3 Cd1 101.0(6) . 2_665 ?
C1 O1 Cd1 108.2(6) . . ?
C9 O5 Cd1 98.6(6) . 2_656 ?
C3 N1 Cd1 105.9(6) . . ?
C3 N1 C2 123.2(8) . . ?
C2 N1 Cd1 103.4(5) . . ?
C1 O2 Cd2 117.3(6) . 1_645 ?
Cd2 O6 Cd1 99.5(3) 1_546 2_656 ?
C9 O6 Cd2 173.3(7) . 1_546 ?
C9 O6 Cd1 86.1(7) . 2_656 ?
C10 C8 C9 117.9(8) . . ?
C10 C8 C7 120.9(9) . . ?
C7 C8 C9 120.8(9) . . ?
O5 C9 Cd1 53.8(5) . 2_656 ?
O5 C9 C8 119.0(8) . . ?
O6 C9 Cd1 66.7(6) . 2_656 ?
O6 C9 O5 120.3(9) . . ?
O6 C9 C8 120.7(10) . . ?
C8 C9 Cd1 170.1(7) . 2_656 ?
C3 C4 C5 118.6(9) . . ?
C4 C3 N1 123.2(9) . . ?
C4 C3 C10 120.3(9) . . ?
C10 C3 N1 116.0(8) . . ?
N1 C2 C1 108.9(7) . . ?
O4 C6 O3 120.1(8) . . ?
O4 C6 C5 120.3(8) . . ?
O3 C6 C5 119.5(9) . . ?
C4 C5 C6 119.6(8) . . ?
C7 C5 C4 122.1(8) . . ?
C7 C5 C6 118.1(8) . . ?
C8 C10 C3 120.0(8) . . ?
C5 C7 C8 117.9(9) . . ?
O1 C1 O2 124.6(9) . . ?
O1 C1 C2 118.2(8) . . ?
O2 C1 C2 117.2(8) . . ?





# start Validation Reply Form
_vrf_PLAT029_s18adb31            
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.915 Why?
RESPONSE: The diffraction pattern was not of premium quality. The 
data were integrated initially to take account of twinning, 
but the level of peak overlap rendered it difficult to 
de-convolute the component intensity data . Ultimately, 
the raw data were integrated by increasing the integration 
mask (1.5 x default mask size) and profile size altering 
with incident angle. Essentially, this treated split peaks 
as arising from a slightly cracked crystal rather than a 
well-defined twin. The latter approach gave the most 
satisfactory residuals and Rint. A side by side comparison 
of the outputs from both data treatments showed that the 
optimal one chosen did not negatively impact on the esds 
associated with the bond/angle metrics. The completeness 
of the data is less than ideal, but the structure is unambiguous.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_s19adb24
_database_code_depnum_ccdc_archive 'CCDC 2097433'
loop_
_audit_author_name
_audit_author_address
'Mary Mahon'
;University of Bath
United Kingdom
;
_audit_update_record             
;
2021-07-19 deposited with the CCDC.	2021-12-20 downloaded from the CCDC.
;
_audit_creation_date             2019-11-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C20 H18 Cd3 N2 O15, 6(H2 O)'
_chemical_formula_sum            'C20 H30 Cd3 N2 O21'
_chemical_formula_weight         971.66
_chemical_absolute_configuration syn
_chemical_melting_point          ?
_chemical_oxdiff_usercomment     'Colourless Plate'
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'
Cd Cd 0.1185 4.6533 '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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   9.01260(10)
_cell_length_b                   18.66240(10)
_cell_length_c                   9.16440(10)
_cell_angle_alpha                90
_cell_angle_beta                 103.4670(10)
_cell_angle_gamma                90
_cell_volume                     1499.04(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9216
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.8850
_cell_measurement_theta_min      4.9770
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    17.751
_exptl_absorpt_correction_T_max  0.36679
_exptl_absorpt_correction_T_min  0.29390
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.153
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.218
_exptl_crystal_size_mid          0.104
_exptl_crystal_size_min          0.036
_exptl_crystal_size_rad          0.055
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0376
_diffrn_reflns_av_unetI/netI     0.0439
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            10096
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.052
_diffrn_reflns_theta_min         4.739
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1150
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.938
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                5338
_reflns_number_total             5352
_reflns_special_details          
;

The compound s19adb24 crystallises in the space group P21 as a racemic twin.
 The asymmetric unit contains three cadmium centres, two 5-CMAI linkers, 
three water ligands and a total of 6 guest water molecules. Interactions 
from the flexible arm of the linkers and the cadmium centres form 1-D chains 
running in the direction of the c-axis. The rest of the 5-CMAI linkers bridge 
the 1-D chains together creating channels running in the c-axis, in which the 
guest water molecules reside. The hydrogen atoms on the water molecules and 
amine of 5-CMAI were included at calculated positions and were corroborated 
by the formation of an extensive hydrogen bonding network. 

 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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         2.097
_refine_diff_density_min         -1.132
_refine_diff_density_rms         0.191
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.426(12)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     449
_refine_ls_number_reflns         5352
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0418
_refine_ls_restrained_S_all      1.072
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0796P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1045
_refine_ls_wR_factor_ref         0.1045
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.574(12)
 0.426(12)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups, All O(H,H,H,H) groups
3. Restrained distances
 N1-H1
 0.98 with sigma of 0.005
 N2-H2
 0.98 with sigma of 0.005
4. Others
 Fixed Sof: O21A(0.5) H21A(0.5) H21B(0.5) O21B(0.5) H21C(0.5) H21D(0.5)
5.a Free rotating group:
 O16(H16A,H16B), O17(H17A,H17B), O18(H18A,H18B), O19(H19A,H19B), O20(H20A,
 H20B), O21A(H1,H2,H21A,H21B), O21B(H21C,H21D)
5.b Rotating group:
 O13(H13A,H13B), O14(H14A,H14B), O15(H15A,H15B)
5.c Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C12(H12A,H12B)
5.d Aromatic/amide H refined with riding coordinates:
 C4(H4), C7(H7), C10(H10), C14(H14), C17(H17), C20(H20)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.60843(6) 0.41539(3) 0.60524(6) 0.01343(16) Uani 1 1 d . . . . .
Cd2 Cd 0.77041(7) 0.53998(3) 1.18179(7) 0.01589(17) Uani 1 1 d . . . . .
Cd3 Cd 0.21817(6) 0.86800(3) 1.02420(6) 0.01292(15) Uani 1 1 d . . . . .
O1 O 0.6351(8) 0.4535(4) 0.3774(8) 0.0204(14) Uani 1 1 d . . . . .
O2 O 0.7033(8) 0.4232(4) 0.1695(8) 0.0189(13) Uani 1 1 d . . . . .
O3 O 0.3254(7) 0.1156(4) 0.6777(8) 0.0184(13) Uani 1 1 d . . . . .
O4 O 0.0805(8) 0.1175(4) 0.5655(9) 0.0245(15) Uani 1 1 d . . . . .
O5 O -0.0908(7) 0.2827(4) 0.1393(8) 0.0202(14) Uani 1 1 d . . . . .
O6 O 0.0491(7) 0.3752(4) 0.1060(7) 0.0183(13) Uani 1 1 d . . . . .
O7 O 0.8099(8) 0.4873(4) 0.9441(8) 0.0162(13) Uani 1 1 d . . . . .
O8 O 0.7124(9) 0.5167(4) 0.7044(8) 0.0218(15) Uani 1 1 d . . . . .
O9 O 1.2047(7) 0.8387(4) 1.2598(7) 0.0168(13) Uani 1 1 d . . . . .
O10 O 1.0821(8) 0.8780(4) 1.4275(9) 0.0263(16) Uani 1 1 d . . . . .
O11 O 0.5074(8) 0.8779(4) 1.2047(8) 0.0214(15) Uani 1 1 d . . . . .
O12 O 0.4118(7) 0.7899(4) 1.0476(7) 0.0151(13) Uani 1 1 d . . . . .
O13 O 0.3748(8) 0.4663(4) 0.5145(9) 0.0277(17) Uani 1 1 d . . . . .
H13A H 0.381682 0.511122 0.479847 0.042 Uiso 1 1 d GR . . . .
H13B H 0.324653 0.473814 0.587530 0.042 Uiso 1 1 d GR . . . .
O14 O 1.0193(8) 0.4999(4) 1.2608(8) 0.0235(15) Uani 1 1 d . . . . .
H14A H 1.087192 0.534693 1.258208 0.035 Uiso 1 1 d GR . . . .
H14B H 1.042013 0.467423 1.197225 0.035 Uiso 1 1 d GR . . . .
O15 O 0.5211(8) 0.5485(4) 1.0131(10) 0.0277(16) Uani 1 1 d . . . . .
H15A H 0.460796 0.518111 1.039188 0.042 Uiso 1 1 d GR . . . .
H15B H 0.526016 0.535030 0.924938 0.042 Uiso 1 1 d GR . . . .
N1 N 0.5771(8) 0.3112(4) 0.4445(9) 0.0158(15) Uani 1 1 d D . . . .
N2 N 0.8588(8) 0.6260(4) 1.0342(9) 0.0150(15) Uani 1 1 d D . . . .
C1 C 0.6570(9) 0.4071(5) 0.2867(10) 0.0152(18) Uani 1 1 d . . . . .
C2 C 0.6338(10) 0.3279(5) 0.3096(10) 0.0153(17) Uani 1 1 d . . . . .
H2A H 0.561851 0.309397 0.222134 0.018 Uiso 1 1 calc R . . . .
H2B H 0.730079 0.303355 0.316855 0.018 Uiso 1 1 calc R . . . .
C3 C 0.4247(10) 0.2842(5) 0.4178(10) 0.0149(17) Uani 1 1 d . . . . .
C4 C 0.3074(10) 0.3141(5) 0.3092(10) 0.0150(17) Uani 1 1 d . . . . .
H4 H 0.326946 0.352039 0.250527 0.018 Uiso 1 1 calc R . . . .
C5 C 0.1601(11) 0.2868(5) 0.2890(11) 0.0175(19) Uani 1 1 d . . . . .
C6 C 0.0335(10) 0.3169(5) 0.1715(11) 0.0170(18) Uani 1 1 d . . . . .
C7 C 0.1291(10) 0.2313(5) 0.3797(10) 0.0158(18) Uani 1 1 d . . . . .
H7 H 0.030056 0.214041 0.366924 0.019 Uiso 1 1 calc R . . . .
C8 C 0.2444(10) 0.2023(5) 0.4870(10) 0.0150(17) Uani 1 1 d . . . . .
C9 C 0.2140(11) 0.1404(6) 0.5815(12) 0.0188(19) Uani 1 1 d . . . . .
C10 C 0.3930(10) 0.2286(5) 0.5084(10) 0.0147(17) Uani 1 1 d . . . . .
H10 H 0.470771 0.209277 0.582881 0.018 Uiso 1 1 calc R . . . .
C11 C 0.7685(10) 0.5317(5) 0.8387(10) 0.0147(17) Uani 1 1 d . . . . .
C12 C 0.7892(11) 0.6117(5) 0.8756(11) 0.0171(18) Uani 1 1 d . . . . .
H12A H 0.852557 0.632730 0.814627 0.021 Uiso 1 1 calc R . . . .
H12B H 0.690291 0.635025 0.849035 0.021 Uiso 1 1 calc R . . . .
C13 C 0.8415(10) 0.6969(5) 1.0887(10) 0.0140(17) Uani 1 1 d . . . . .
C14 C 0.9686(10) 0.7349(5) 1.1636(11) 0.0170(18) Uani 1 1 d . . . . .
H14 H 1.065924 0.718014 1.164583 0.020 Uiso 1 1 calc R . . . .
C15 C 0.9502(10) 0.7982(5) 1.2374(10) 0.0155(17) Uani 1 1 d . . . . .
C16 C 1.0854(10) 0.8416(5) 1.3158(11) 0.0160(18) Uani 1 1 d . . . . .
C17 C 0.8064(10) 0.8245(5) 1.2357(10) 0.0145(17) Uani 1 1 d . . . . .
H17 H 0.794770 0.865263 1.290360 0.017 Uiso 1 1 calc R . . . .
C18 C 0.6789(10) 0.7890(5) 1.1509(11) 0.0162(18) Uani 1 1 d . . . . .
C19 C 0.5237(10) 0.8198(5) 1.1364(11) 0.0173(18) Uani 1 1 d . . . . .
C20 C 0.6959(10) 0.7255(5) 1.0784(10) 0.0158(18) Uani 1 1 d . . . . .
H20 H 0.610449 0.701823 1.022750 0.019 Uiso 1 1 calc R . . . .
O16 O 0.0925(9) 0.4992(6) 0.5978(13) 0.043(2) Uani 1 1 d . . . . .
H16A H 0.031045 0.532268 0.559131 0.065 Uiso 1 1 d G . . . .
H16B H 0.042068 0.473586 0.646006 0.065 Uiso 1 1 d G . . . .
O17 O 0.3722(8) 0.5877(5) 0.3439(9) 0.0272(16) Uani 1 1 d . . . . .
H17A H 0.305293 0.591177 0.261924 0.041 Uiso 1 1 d G . . . .
H17B H 0.456883 0.591608 0.318803 0.041 Uiso 1 1 d G . . . .
O18 O 0.2297(9) 0.6720(5) 0.5315(10) 0.0300(18) Uani 1 1 d . . . . .
H18A H 0.287617 0.639645 0.510122 0.045 Uiso 1 1 d G . . . .
H18B H 0.143722 0.664391 0.471737 0.045 Uiso 1 1 d G . . . .
O19 O 0.3428(9) 0.6618(5) 0.8525(10) 0.0313(17) Uani 1 1 d . . . . .
H19A H 0.281866 0.662441 0.766385 0.047 Uiso 1 1 d G . . . .
H19B H 0.415288 0.634631 0.841910 0.047 Uiso 1 1 d G . . . .
O20 O 0.1800(9) 0.5993(5) 1.0519(11) 0.036(2) Uani 1 1 d . . . . .
H20A H 0.219004 0.625882 0.995437 0.054 Uiso 1 1 d G . . . .
H20B H 0.186292 0.557132 1.018718 0.054 Uiso 1 1 d G . . . .
O21A O 0.212(3) 0.4712(14) 0.949(3) 0.040(6) Uani 0.5 1 d . . P A 1
H1 H 0.648361 0.273049 0.488097 0.060 Uiso 1 1 d DG . . . .
H2 H 0.964821 0.609178 1.057400 0.060 Uiso 1 1 d DG . . . .
H21A H 0.200079 0.434299 0.999376 0.060 Uiso 0.5 1 d G . P A 1
H21B H 0.168530 0.460679 0.859036 0.060 Uiso 0.5 1 d G . P A 1
O21B O 0.268(3) 0.4523(15) 0.996(4) 0.045(6) Uani 0.5 1 d . . P B 2
H21C H 0.193895 0.431028 1.020545 0.068 Uiso 0.5 1 d G . P B 2
H21D H 0.314463 0.419361 0.960765 0.068 Uiso 0.5 1 d G . P B 2


_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 O1 2.271(7) . ?
Cd1 O8 2.210(7) . ?
Cd1 O9 2.334(7) 2_747 ?
Cd1 O11 2.337(7) 2_647 ?
Cd1 O13 2.283(7) . ?
Cd1 N1 2.415(8) . ?
Cd2 O2 2.258(7) 1_556 ?
Cd2 O3 2.217(6) 2_657 ?
Cd2 O7 2.490(7) . ?
Cd2 O14 2.315(7) . ?
Cd2 O15 2.417(7) . ?
Cd2 N2 2.355(8) . ?
Cd3 O2 2.301(7) 2_656 ?
Cd3 O5 2.301(7) 2_556 ?
Cd3 O6 2.430(6) 2_556 ?
Cd3 O7 2.266(7) 2_657 ?
Cd3 O9 2.258(6) 1_455 ?
Cd3 O12 2.246(6) . ?
Cd3 C6 2.716(9) 2_556 ?
O1 C1 1.247(12) . ?
O2 C1 1.276(11) . ?
O3 C9 1.259(12) . ?
O4 C9 1.252(12) . ?
O5 C6 1.263(12) . ?
O6 C6 1.267(13) . ?
O7 C11 1.261(12) . ?
O8 C11 1.249(12) . ?
O9 C16 1.296(12) . ?
O10 C16 1.235(13) . ?
O11 C19 1.277(13) . ?
O12 C19 1.269(12) . ?
O13 H13A 0.9016 . ?
O13 H13B 0.9015 . ?
O14 H14A 0.8968 . ?
O14 H14B 0.8969 . ?
O15 H15A 0.8568 . ?
O15 H15B 0.8570 . ?
N1 C2 1.477(11) . ?
N1 C3 1.430(12) . ?
N1 H1 0.9799 . ?
N2 C12 1.467(12) . ?
N2 C13 1.436(12) . ?
N2 H2 0.9805 . ?
C1 C2 1.514(14) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.390(13) . ?
C3 C10 1.399(13) . ?
C4 H4 0.9300 . ?
C4 C5 1.393(13) . ?
C5 C6 1.485(13) . ?
C5 C7 1.397(14) . ?
C7 H7 0.9300 . ?
C7 C8 1.366(13) . ?
C8 C9 1.507(14) . ?
C8 C10 1.397(13) . ?
C10 H10 0.9300 . ?
C11 C12 1.534(13) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C14 1.385(13) . ?
C13 C20 1.399(13) . ?
C14 H14 0.9300 . ?
C14 C15 1.391(14) . ?
C15 C16 1.499(12) . ?
C15 C17 1.383(13) . ?
C17 H17 0.9300 . ?
C17 C18 1.395(13) . ?
C18 C19 1.489(12) . ?
C18 C20 1.385(14) . ?
C20 H20 0.9300 . ?
O16 H16A 0.8499 . ?
O16 H16B 0.8500 . ?
O17 H17A 0.8496 . ?
O17 H17B 0.8500 . ?
O18 H18A 0.8503 . ?
O18 H18B 0.8500 . ?
O19 H19A 0.8499 . ?
O19 H19B 0.8498 . ?
O20 H20A 0.8502 . ?
O20 H20B 0.8503 . ?
O21A H21A 0.8500 . ?
O21A H21B 0.8501 . ?
O21B H21C 0.8496 . ?
O21B H21D 0.8502 . ?

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
O1 Cd1 O9 117.5(2) . 2_747 ?
O1 Cd1 O11 160.1(3) . 2_647 ?
O1 Cd1 O13 79.7(3) . . ?
O1 Cd1 N1 73.4(3) . . ?
O8 Cd1 O1 89.1(3) . . ?
O8 Cd1 O9 97.0(3) . 2_747 ?
O8 Cd1 O11 99.8(3) . 2_647 ?
O8 Cd1 O13 93.5(3) . . ?
O8 Cd1 N1 156.6(3) . . ?
O9 Cd1 O11 79.3(2) 2_747 2_647 ?
O9 Cd1 N1 78.3(2) 2_747 . ?
O11 Cd1 N1 101.8(3) 2_647 . ?
O13 Cd1 O9 159.9(3) . 2_747 ?
O13 Cd1 O11 82.1(3) . 2_647 ?
O13 Cd1 N1 98.4(3) . . ?
O2 Cd2 O7 70.5(2) 1_556 . ?
O2 Cd2 O14 86.1(3) 1_556 . ?
O2 Cd2 O15 80.4(3) 1_556 . ?
O2 Cd2 N2 138.8(3) 1_556 . ?
O3 Cd2 O2 120.5(3) 2_657 1_556 ?
O3 Cd2 O7 156.1(2) 2_657 . ?
O3 Cd2 O14 120.3(3) 2_657 . ?
O3 Cd2 O15 84.3(3) 2_657 . ?
O3 Cd2 N2 97.4(3) 2_657 . ?
O14 Cd2 O7 79.7(2) . . ?
O14 Cd2 O15 155.5(3) . . ?
O14 Cd2 N2 88.1(3) . . ?
O15 Cd2 O7 76.5(3) . . ?
N2 Cd2 O7 68.3(3) . . ?
N2 Cd2 O15 88.7(3) . . ?
O2 Cd3 O5 90.2(3) 2_656 2_556 ?
O2 Cd3 O6 92.5(2) 2_656 2_556 ?
O2 Cd3 C6 90.4(3) 2_656 2_556 ?
O5 Cd3 O6 55.4(2) 2_556 2_556 ?
O5 Cd3 C6 27.6(3) 2_556 2_556 ?
O6 Cd3 C6 27.8(3) 2_556 2_556 ?
O7 Cd3 O2 73.9(2) 2_657 2_656 ?
O7 Cd3 O5 135.2(2) 2_657 2_556 ?
O7 Cd3 O6 83.2(2) 2_657 2_556 ?
O7 Cd3 C6 109.2(3) 2_657 2_556 ?
O9 Cd3 O2 160.2(2) 1_455 2_656 ?
O9 Cd3 O5 109.0(3) 1_455 2_556 ?
O9 Cd3 O6 102.4(2) 1_455 2_556 ?
O9 Cd3 O7 94.8(3) 1_455 2_657 ?
O9 Cd3 C6 108.9(3) 1_455 2_556 ?
O12 Cd3 O2 89.6(2) . 2_656 ?
O12 Cd3 O5 82.6(2) . 2_556 ?
O12 Cd3 O6 137.9(2) . 2_556 ?
O12 Cd3 O7 137.1(2) . 2_657 ?
O12 Cd3 O9 88.0(2) . 1_455 ?
O12 Cd3 C6 110.2(3) . 2_556 ?
C1 O1 Cd1 117.5(6) . . ?
Cd2 O2 Cd3 110.1(3) 1_554 2_646 ?
C1 O2 Cd2 108.7(6) . 1_554 ?
C1 O2 Cd3 139.9(7) . 2_646 ?
C9 O3 Cd2 106.6(6) . 2_647 ?
C6 O5 Cd3 94.8(6) . 2_546 ?
C6 O6 Cd3 88.7(5) . 2_546 ?
Cd3 O7 Cd2 103.5(2) 2_647 . ?
C11 O7 Cd2 109.4(6) . . ?
C11 O7 Cd3 136.2(6) . 2_647 ?
C11 O8 Cd1 129.2(6) . . ?
Cd3 O9 Cd1 99.5(2) 1_655 2_757 ?
C16 O9 Cd1 109.1(6) . 2_757 ?
C16 O9 Cd3 127.1(6) . 1_655 ?
C19 O11 Cd1 137.9(6) . 2_657 ?
C19 O12 Cd3 105.0(6) . . ?
Cd1 O13 H13A 112.4 . . ?
Cd1 O13 H13B 111.9 . . ?
H13A O13 H13B 101.8 . . ?
Cd2 O14 H14A 112.0 . . ?
Cd2 O14 H14B 111.5 . . ?
H14A O14 H14B 102.2 . . ?
Cd2 O15 H15A 109.5 . . ?
Cd2 O15 H15B 109.9 . . ?
H15A O15 H15B 104.2 . . ?
Cd1 N1 H1 111.4 . . ?
C2 N1 Cd1 109.0(6) . . ?
C2 N1 H1 99.9 . . ?
C3 N1 Cd1 111.1(6) . . ?
C3 N1 C2 115.9(7) . . ?
C3 N1 H1 109.0 . . ?
Cd2 N2 H2 95.7 . . ?
C12 N2 Cd2 108.7(5) . . ?
C12 N2 H2 109.1 . . ?
C13 N2 Cd2 110.5(5) . . ?
C13 N2 C12 117.1(7) . . ?
C13 N2 H2 113.5 . . ?
O1 C1 O2 122.2(9) . . ?
O1 C1 C2 122.5(8) . . ?
O2 C1 C2 115.4(8) . . ?
N1 C2 C1 114.1(7) . . ?
N1 C2 H2A 108.7 . . ?
N1 C2 H2B 108.7 . . ?
C1 C2 H2A 108.7 . . ?
C1 C2 H2B 108.7 . . ?
H2A C2 H2B 107.6 . . ?
C4 C3 N1 121.4(9) . . ?
C4 C3 C10 119.8(8) . . ?
C10 C3 N1 118.7(8) . . ?
C3 C4 H4 120.3 . . ?
C3 C4 C5 119.4(9) . . ?
C5 C4 H4 120.3 . . ?
C4 C5 C6 120.3(9) . . ?
C4 C5 C7 120.6(9) . . ?
C7 C5 C6 119.0(8) . . ?
O5 C6 Cd3 57.6(5) . 2_546 ?
O5 C6 O6 120.9(9) . . ?
O5 C6 C5 117.9(9) . . ?
O6 C6 Cd3 63.5(5) . 2_546 ?
O6 C6 C5 121.1(9) . . ?
C5 C6 Cd3 173.9(7) . 2_546 ?
C5 C7 H7 120.1 . . ?
C8 C7 C5 119.9(8) . . ?
C8 C7 H7 120.1 . . ?
C7 C8 C9 120.5(9) . . ?
C7 C8 C10 120.4(9) . . ?
C10 C8 C9 119.1(8) . . ?
O3 C9 C8 117.5(9) . . ?
O4 C9 O3 123.0(10) . . ?
O4 C9 C8 119.5(9) . . ?
C3 C10 H10 120.0 . . ?
C8 C10 C3 120.0(8) . . ?
C8 C10 H10 120.0 . . ?
O7 C11 C12 118.2(8) . . ?
O8 C11 O7 126.0(9) . . ?
O8 C11 C12 115.8(8) . . ?
N2 C12 C11 113.4(8) . . ?
N2 C12 H12A 108.9 . . ?
N2 C12 H12B 108.9 . . ?
C11 C12 H12A 108.9 . . ?
C11 C12 H12B 108.9 . . ?
H12A C12 H12B 107.7 . . ?
C14 C13 N2 119.9(8) . . ?
C14 C13 C20 119.5(9) . . ?
C20 C13 N2 120.3(8) . . ?
C13 C14 H14 120.1 . . ?
C13 C14 C15 119.8(8) . . ?
C15 C14 H14 120.1 . . ?
C14 C15 C16 121.1(8) . . ?
C17 C15 C14 120.9(8) . . ?
C17 C15 C16 117.9(9) . . ?
O9 C16 C15 116.4(9) . . ?
O10 C16 O9 122.2(9) . . ?
O10 C16 C15 121.4(9) . . ?
C15 C17 H17 120.5 . . ?
C15 C17 C18 119.1(9) . . ?
C18 C17 H17 120.5 . . ?
C17 C18 C19 120.1(9) . . ?
C20 C18 C17 120.3(8) . . ?
C20 C18 C19 119.6(8) . . ?
O11 C19 C18 119.8(9) . . ?
O12 C19 O11 121.6(8) . . ?
O12 C19 C18 118.5(9) . . ?
C13 C20 H20 120.0 . . ?
C18 C20 C13 120.0(8) . . ?
C18 C20 H20 120.0 . . ?
H16A O16 H16B 104.5 . . ?
H17A O17 H17B 104.5 . . ?
H18A O18 H18B 104.5 . . ?
H19A O19 H19B 104.5 . . ?
H20A O20 H20B 104.5 . . ?
H21A O21A H21B 104.5 . . ?
H21C O21B H21D 104.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O13 H13A O17 0.90 1.88 2.748(12) 160.0 .
O13 H13B O16 0.90 2.17 2.888(11) 136.2 .
O14 H14B O6 0.90 1.92 2.770(11) 157.5 1_656
O15 H15A O21B 0.86 2.09 2.88(3) 152.9 .
O16 H16A O4 0.85 2.08 2.909(13) 166.2 2_556
O16 H16B O10 0.85 2.13 2.733(12) 127.7 2_647
O17 H17A O20 0.85 2.00 2.838(13) 169.7 1_554
O17 H17B O3 0.85 2.01 2.827(10) 162.1 2_656
O18 H18A O17 0.85 2.09 2.848(12) 147.5 .
O19 H19A O18 0.85 2.10 2.886(13) 153.4 .
O19 H19B O15 0.85 2.29 2.850(12) 123.3 .
O20 H20A O19 0.85 2.02 2.847(13) 163.1 .
O20 H20B O21A 0.85 1.76 2.61(3) 176.0 .
O21B H21C O6 0.85 1.97 2.81(3) 170.1 1_556

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.574(12)
2 0.426(12)
####################################################################### 
# 
# 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_s18adb20
_database_code_depnum_ccdc_archive 'CCDC 2097434'
loop_
_audit_author_name
_audit_author_address
'Mary Mahon'
;University of Bath
United Kingdom
;
_audit_update_record             
;
2021-07-19 deposited with the CCDC.	2021-12-20 downloaded from the CCDC.
;
_audit_creation_date             2018-08-09
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelxl_version_number           2014-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C10 H11 N O8 Zn'
_chemical_formula_sum            'C10 H11 N O8 Zn'
_chemical_formula_weight         338.57
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_usercomment     'Colourless crystal'
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'
Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   4.89590(10)
_cell_length_b                   10.0630(3)
_cell_length_c                   11.3009(4)
_cell_angle_alpha                90
_cell_angle_beta                 95.584(3)
_cell_angle_gamma                90
_cell_volume                     554.12(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2901
_cell_measurement_temperature    149.9(3)
_cell_measurement_theta_max      73.1370
_cell_measurement_theta_min      3.9660
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.538
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81015
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.029
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             344
_exptl_crystal_size_max          0.141
_exptl_crystal_size_mid          0.041
_exptl_crystal_size_min          0.023
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_unetI/netI     0.0320
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4616
_diffrn_reflns_point_group_measured_fraction_full 0.740
_diffrn_reflns_point_group_measured_fraction_max 0.732
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.411
_diffrn_reflns_theta_min         3.930
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.9(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1150
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.382
_reflns_Friedel_fraction_full    0.446
_reflns_Friedel_fraction_max     0.431
_reflns_number_gt                1604
_reflns_number_total             1628
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.660
_refine_diff_density_min         -0.490
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details 
;
 Flack x determined using 440 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.09(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     189
_refine_ls_number_reflns         1628
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0308
_refine_ls_restrained_S_all      1.068
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0492P)²+0.4235P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0803
_refine_ls_wR_factor_ref         0.0810
_refine_special_details          
;
The asymmetric unit in this structure contains one full zinc centre, 
one H-5-CMAI ligand and two co-ordinated water ligands. H1, attached 
to N1, was readily found and refined subject to being located at a 
distance of 0.98 Å from its parent. All other hydrogens (including 
the carboxylic acid hydrogen, H6) were included at calculated 
positions. The Uiso values for H1 and H6 were refined freely.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 N1-H1
 0.98 with sigma of 0.005
3.a Rotating group:
 O7(H7A,H7B), O8(H8A,H8B)
3.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B)
3.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C7(H7), C10(H10)
3.d Idealised tetrahedral OH refined as rotating group:
 O6(H6)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
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 0.62902(9) 0.24928(7) 0.77052(5) 0.01482(17) Uani 1 1 d . . . . .
O1 O 0.3975(6) 0.2913(3) 0.6095(3) 0.0184(7) Uani 1 1 d . . . . .
O2 O 0.4030(7) 0.4043(4) 0.4417(3) 0.0262(8) Uani 1 1 d . . . . .
O3 O 1.0887(6) 0.7148(3) 1.0917(3) 0.0191(8) Uani 1 1 d . . . . .
O4 O 0.7056(6) 0.8078(3) 1.1446(3) 0.0149(6) Uani 1 1 d . . . . .
O5 O 0.0294(9) 0.9024(5) 0.7880(4) 0.0447(13) Uani 1 1 d . . . . .
O6 O 0.0026(6) 0.7590(5) 0.6377(3) 0.0195(7) Uani 1 1 d . . . . .
H6 H -0.1230 0.8079 0.6116 0.06(3) Uiso 1 1 calc GR . . . .
O7 O 0.5185(13) 0.0551(5) 0.7724(7) 0.0653(18) Uani 1 1 d . . . . .
H7A H 0.6329 0.0073 0.7375 0.098 Uiso 1 1 d GR . . . .
H7B H 0.3651 0.0439 0.7293 0.098 Uiso 1 1 d GR . . . .
O8 O 0.9145(9) 0.1534(5) 0.6465(4) 0.0385(10) Uani 1 1 d . . . . .
H8A H 1.0023 0.0835 0.6802 0.058 Uiso 1 1 d GR . . . .
H8B H 1.0517 0.2076 0.6332 0.058 Uiso 1 1 d GR . . . .
N1 N 0.7977(7) 0.4418(4) 0.7256(3) 0.0125(7) Uani 1 1 d D . . . .
H1 H 0.977(7) 0.447(8) 0.772(6) 0.04(2) Uiso 1 1 d D . . . .
C1 C 0.4991(9) 0.3761(5) 0.5450(4) 0.0162(9) Uani 1 1 d . . . . .
C2 C 0.7600(8) 0.4481(5) 0.5946(4) 0.0144(8) Uani 1 1 d . . . . .
H2A H 0.9172 0.4080 0.5625 0.017 Uiso 1 1 calc R . . . .
H2B H 0.7501 0.5404 0.5696 0.017 Uiso 1 1 calc R . . . .
C3 C 0.6820(8) 0.5495(5) 0.7864(4) 0.0111(8) Uani 1 1 d . . . . .
C4 C 0.8021(8) 0.5868(5) 0.8985(4) 0.0125(8) Uani 1 1 d . . . . .
H4 H 0.9534 0.5405 0.9336 0.015 Uiso 1 1 calc R . . . .
C5 C 0.6952(9) 0.6937(5) 0.9583(4) 0.0134(8) Uani 1 1 d . . . . .
C6 C 0.8392(8) 0.7402(6) 1.0739(3) 0.0132(8) Uani 1 1 d . . . . .
C7 C 0.4680(8) 0.7627(6) 0.9068(4) 0.0136(8) Uani 1 1 d . . . . .
H7 H 0.3967 0.8336 0.9467 0.016 Uiso 1 1 calc R . . . .
C8 C 0.3480(8) 0.7250(4) 0.7954(4) 0.0131(10) Uani 1 1 d . . . . .
C9 C 0.1114(9) 0.8046(5) 0.7394(5) 0.0183(9) Uani 1 1 d . . . . .
C10 C 0.4518(9) 0.6184(4) 0.7354(4) 0.0124(8) Uani 1 1 d . . . . .
H10 H 0.3681 0.5929 0.6614 0.015 Uiso 1 1 calc R . . . .


_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 O1 2.091(3) . ?
Zn1 O3 2.009(3) 2_747 ?
Zn1 O4 2.063(3) 2_647 ?
Zn1 O7 2.028(5) . ?
Zn1 O8 2.286(4) . ?
Zn1 N1 2.185(4) . ?
O1 C1 1.257(6) . ?
O2 C1 1.248(6) . ?
O3 Zn1 2.009(3) 2_757 ?
O3 C6 1.245(5) . ?
O4 Zn1 2.063(3) 2_657 ?
O4 C6 1.278(6) . ?
O5 C9 1.214(7) . ?
O6 C9 1.303(6) . ?
N1 C2 1.475(5) . ?
N1 C3 1.430(6) . ?
C1 C2 1.527(6) . ?
C3 C4 1.396(6) . ?
C3 C10 1.399(6) . ?
C4 C5 1.399(7) . ?
C5 C6 1.497(6) . ?
C5 C7 1.390(6) . ?
C7 C8 1.390(6) . ?
C8 C9 1.497(6) . ?
C8 C10 1.392(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
O1 Zn1 O8 82.18(15) . . ?
O1 Zn1 N1 78.67(13) . . ?
O3 Zn1 O1 169.43(12) 2_747 . ?
O3 Zn1 O4 101.93(13) 2_747 2_647 ?
O3 Zn1 O7 89.4(2) 2_747 . ?
O3 Zn1 O8 89.23(15) 2_747 . ?
O3 Zn1 N1 94.94(14) 2_747 . ?
O4 Zn1 O1 87.64(13) 2_647 . ?
O4 Zn1 O8 164.94(15) 2_647 . ?
O4 Zn1 N1 100.96(14) 2_647 . ?
O7 Zn1 O1 94.7(2) . . ?
O7 Zn1 O4 92.61(19) . 2_647 ?
O7 Zn1 O8 77.3(2) . . ?
O7 Zn1 N1 164.5(2) . . ?
N1 Zn1 O8 87.94(16) . . ?
C1 O1 Zn1 115.5(3) . . ?
C6 O3 Zn1 132.9(3) . 2_757 ?
C6 O4 Zn1 128.1(3) . 2_657 ?
C2 N1 Zn1 105.0(3) . . ?
C3 N1 Zn1 112.6(3) . . ?
C3 N1 C2 115.7(4) . . ?
O1 C1 C2 118.3(4) . . ?
O2 C1 O1 124.2(4) . . ?
O2 C1 C2 117.5(4) . . ?
N1 C2 C1 111.5(4) . . ?
C4 C3 N1 119.3(4) . . ?
C4 C3 C10 119.5(4) . . ?
C10 C3 N1 121.2(4) . . ?
C3 C4 C5 120.1(4) . . ?
C4 C5 C6 119.7(4) . . ?
C7 C5 C4 120.2(4) . . ?
C7 C5 C6 119.9(4) . . ?
O3 C6 O4 124.2(4) . . ?
O3 C6 C5 116.7(4) . . ?
O4 C6 C5 119.1(4) . . ?
C5 C7 C8 119.6(4) . . ?
C7 C8 C9 118.6(4) . . ?
C7 C8 C10 120.7(4) . . ?
C10 C8 C9 120.7(4) . . ?
O5 C9 O6 124.1(5) . . ?
O5 C9 C8 121.3(5) . . ?
O6 C9 C8 114.7(4) . . ?
C8 C10 C3 119.9(4) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O6 H6 O1 0.82 2.73 3.269(4) 125.3 2_556
O6 H6 O2 0.82 1.74 2.558(5) 176.6 2_556
O7 H7A O2 0.86 2.27 2.913(8) 131.8 2_646
O7 H7A O5 0.86 2.23 2.926(7) 137.2 1_645
O7 H7B O5 0.86 2.32 2.865(8) 121.4 1_545
O8 H8A O5 0.89 2.19 3.014(7) 153.7 1_645
O8 H8B O1 0.89 1.93 2.808(6) 167.7 1_655
N1 H1 O4 0.980(6) 2.23(6) 3.032(5) 138(6) 2_747


_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_s18adb33
_database_code_depnum_ccdc_archive 'CCDC 2097436'
loop_
_audit_author_name
_audit_author_address
'Mary Mahon'
;University of Bath
United Kingdom
;
_audit_update_record             
;
2021-07-19 deposited with the CCDC.	2021-12-20 downloaded from the CCDC.
;
_audit_creation_date             2019-01-08
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelxl_version_number           2014-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C10 H11 Co N O8'
_chemical_formula_sum            'C10 H11 Co N O8'
_chemical_formula_weight         332.13
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_usercomment     'Pink Rod'
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'
Co Co -2.3653 3.6143 '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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   4.8412(2)
_cell_length_b                   10.1675(4)
_cell_length_c                   11.3320(4)
_cell_angle_alpha                90
_cell_angle_beta                 95.158(4)
_cell_angle_gamma                90
_cell_volume                     555.54(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1467
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.1930
_cell_measurement_theta_min      4.0170
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    12.568
_exptl_absorpt_correction_T_max  0.32408
_exptl_absorpt_correction_T_min  0.24298
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.986
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             338
_exptl_crystal_size_max          0.183
_exptl_crystal_size_mid          0.046
_exptl_crystal_size_min          0.033
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_unetI/netI     0.0444
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2451
_diffrn_reflns_point_group_measured_fraction_full 0.755
_diffrn_reflns_point_group_measured_fraction_max 0.743
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.255
_diffrn_reflns_theta_min         3.917
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1150
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.406
_reflns_Friedel_fraction_full    0.480
_reflns_Friedel_fraction_max     0.456
_reflns_number_gt                1586
_reflns_number_total             1637
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.687
_refine_diff_density_min         -0.610
_refine_diff_density_rms         0.099
_refine_ls_abs_structure_details 
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.001(6)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     204
_refine_ls_number_reflns         1637
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0461
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0944P)²+0.0631P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1224
_refine_ls_wR_factor_ref         0.1241
_refine_special_details          
;
The asymmetric unit comprises one cobalt centre, one CMAI 
ligand which is doubly deprotonated and 2 water ligands. 1-dimensional 
polymers dominate the gross structure and these propagate, along b, 
via the 21 screw axis in the space group. The water hydrogens, along 
with those bound to N1 and O6, were located and refined at a distance 
of 0.98Å from the relevant parent atom. Additional distance restraints 
(2.55 Å for Co1...H7a, and 1.5Å for  H7a...H7b) were included, 
to assist convergence. All of these latter hydrogens are 
implicated in the formation of a dense hydrogen-bonded network in 
the lattice. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 O8-H8B = O8-H8A
 0.98 with sigma of 0.005
 H8A-H8B
 1.5 with sigma of 0.005
 O7-H7B = O7-H7A
 0.98 with sigma of 0.005
 H7B-H7A
 1.5 with sigma of 0.005
 Co1-H7B
 2.55 with sigma of 0.005
 O6-H6
 0.98 with sigma of 0.005
 N1-H1
 0.98 with sigma of 0.005
3.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C7(H7), C10(H10)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
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
Co1 Co 1.35864(16) 0.64972(10) 0.73216(6) 0.0152(3) Uani 1 1 d D . . . .
O1 O 0.3951(9) 0.1945(4) 0.1120(4) 0.0202(9) Uani 1 1 d . . . . .
O2 O 0.3876(11) 0.3134(6) -0.0534(4) 0.0334(12) Uani 1 1 d . . . . .
O3 O 1.0764(9) 0.6142(5) 0.5942(3) 0.0218(10) Uani 1 1 d . . . . .
O4 O 0.6894(9) 0.7125(5) 0.6419(4) 0.0198(9) Uani 1 1 d . . . . .
O5 O 0.0205(12) 0.8048(6) 0.2825(5) 0.0415(15) Uani 1 1 d . . . . .
O6 O -0.0039(9) 0.6596(5) 0.1358(3) 0.0211(9) Uani 1 1 d D . . . .
H6 H -0.122(19) 0.729(8) 0.098(9) 0.06(3) Uiso 1 1 d D . . . .
O7 O 1.4883(12) 0.4571(6) 0.7118(6) 0.0411(14) Uani 1 1 d D . . . .
H7A H 1.680(8) 0.426(9) 0.709(7) 0.04(3) Uiso 1 1 d D . . . .
H7B H 1.43(2) 0.407(3) 0.780(5) 0.17(10) Uiso 1 1 d D . . . .
O8 O 1.0903(10) 0.5596(5) 0.8513(4) 0.0232(9) Uani 1 1 d D . . . .
H8A H 0.911(10) 0.579(7) 0.881(8) 0.05(3) Uiso 1 1 d D . . . .
H8B H 1.094(15) 0.4639(12) 0.861(7) 0.03(2) Uiso 1 1 d D . . . .
N1 N 0.7965(10) 0.3462(5) 0.2265(4) 0.0154(10) Uani 1 1 d D . . . .
C1 C 0.4905(12) 0.2827(6) 0.0477(5) 0.0170(11) Uani 1 1 d . . . . .
C2 C 0.7549(12) 0.3526(6) 0.0960(5) 0.0175(11) Uani 1 1 d . . . . .
H2A H 0.9124 0.3126 0.0627 0.021 Uiso 1 1 calc R . . . .
H2B H 0.7458 0.4440 0.0714 0.021 Uiso 1 1 calc R . . . .
C3 C 0.6775(12) 0.4524(6) 0.2882(5) 0.0154(11) Uani 1 1 d . . . . .
C4 C 0.7952(12) 0.4900(6) 0.3986(5) 0.0157(11) Uani 1 1 d . . . . .
H4 H 0.9488 0.4451 0.4334 0.019 Uiso 1 1 calc R . . . .
C5 C 0.6843(12) 0.5958(6) 0.4587(5) 0.0154(11) Uani 1 1 d . . . . .
C6 C 0.8253(11) 0.6426(7) 0.5743(4) 0.0166(10) Uani 1 1 d . . . . .
C7 C 0.4559(11) 0.6640(7) 0.4066(5) 0.0163(11) Uani 1 1 d . . . . .
H7 H 0.3818 0.7341 0.4461 0.020 Uiso 1 1 calc R . . . .
C8 C 0.3391(12) 0.6265(6) 0.2950(5) 0.0171(11) Uani 1 1 d . . . . .
C9 C 0.1035(13) 0.7048(7) 0.2369(6) 0.0199(12) Uani 1 1 d . . . . .
C10 C 0.4465(12) 0.5198(6) 0.2348(5) 0.0156(11) Uani 1 1 d . . . . .
H10 H 0.3655 0.4942 0.1609 0.019 Uiso 1 1 calc R . . . .
H1 H 0.995(4) 0.348(9) 0.252(7) 0.019 Uiso 1 1 d DR . . . .


_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
Co1 O1 2.091(4) 2_756 ?
Co1 O3 2.014(4) . ?
Co1 O4 2.076(4) 1_655 ?
Co1 O7 2.076(6) . ?
Co1 O8 2.160(5) . ?
Co1 N1 2.199(5) 2_756 ?
O1 Co1 2.090(4) 2_746 ?
O1 C1 1.268(8) . ?
O2 C1 1.247(7) . ?
O3 C6 1.250(7) . ?
O4 Co1 2.076(4) 1_455 ?
O4 C6 1.271(7) . ?
O5 C9 1.224(9) . ?
O6 H6 0.979(7) . ?
O6 C9 1.299(8) . ?
O7 H7A 0.980(7) . ?
O7 H7B 0.980(7) . ?
O8 H8A 0.978(7) . ?
O8 H8B 0.979(7) . ?
N1 Co1 2.199(5) 2_746 ?
N1 C2 1.476(7) . ?
N1 C3 1.436(7) . ?
N1 H1 0.980(7) . ?
C1 C2 1.522(8) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.381(8) . ?
C3 C10 1.401(8) . ?
C4 H4 0.9300 . ?
C4 C5 1.405(8) . ?
C5 C6 1.498(7) . ?
C5 C7 1.391(8) . ?
C7 H7 0.9300 . ?
C7 C8 1.391(7) . ?
C8 C9 1.495(8) . ?
C8 C10 1.406(8) . ?
C10 H10 0.9300 . ?

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
O1 Co1 O8 83.91(18) 2_756 . ?
O1 Co1 N1 78.58(17) 2_756 2_756 ?
O3 Co1 O1 172.04(17) . 2_756 ?
O3 Co1 O4 99.92(17) . 1_655 ?
O3 Co1 O7 86.3(2) . . ?
O3 Co1 O8 90.26(18) . . ?
O3 Co1 N1 96.16(18) . 2_756 ?
O4 Co1 O1 86.73(18) 1_655 2_756 ?
O4 Co1 O8 166.42(18) 1_655 . ?
O4 Co1 N1 96.83(19) 1_655 2_756 ?
O7 Co1 O1 98.3(2) . 2_756 ?
O7 Co1 O4 88.9(2) . 1_655 ?
O7 Co1 O8 82.8(2) . . ?
O7 Co1 N1 173.3(2) . 2_756 ?
O8 Co1 N1 90.93(19) . 2_756 ?
C1 O1 Co1 115.5(4) . 2_746 ?
C6 O3 Co1 132.8(4) . . ?
C6 O4 Co1 126.1(4) . 1_455 ?
C9 O6 H6 107(7) . . ?
Co1 O7 H7A 127(6) . . ?
Co1 O7 H7B 107.6(7) . . ?
H7A O7 H7B 99.9(9) . . ?
Co1 O8 H8A 137(5) . . ?
Co1 O8 H8B 119(4) . . ?
H8A O8 H8B 100.1(9) . . ?
Co1 N1 H1 108(5) 2_746 . ?
C2 N1 Co1 103.6(4) . 2_746 ?
C2 N1 H1 109(5) . . ?
C3 N1 Co1 114.8(4) . 2_746 ?
C3 N1 C2 115.5(5) . . ?
C3 N1 H1 106(5) . . ?
O1 C1 C2 117.5(5) . . ?
O2 C1 O1 124.6(5) . . ?
O2 C1 C2 117.9(5) . . ?
N1 C2 C1 112.0(5) . . ?
N1 C2 H2A 109.2 . . ?
N1 C2 H2B 109.2 . . ?
C1 C2 H2A 109.2 . . ?
C1 C2 H2B 109.2 . . ?
H2A C2 H2B 107.9 . . ?
C4 C3 N1 119.9(5) . . ?
C4 C3 C10 120.3(5) . . ?
C10 C3 N1 119.8(5) . . ?
C3 C4 H4 119.8 . . ?
C3 C4 C5 120.4(5) . . ?
C5 C4 H4 119.8 . . ?
C4 C5 C6 120.2(5) . . ?
C7 C5 C4 120.0(5) . . ?
C7 C5 C6 119.7(5) . . ?
O3 C6 O4 124.6(5) . . ?
O3 C6 C5 116.4(5) . . ?
O4 C6 C5 118.9(5) . . ?
C5 C7 H7 120.3 . . ?
C5 C7 C8 119.5(5) . . ?
C8 C7 H7 120.3 . . ?
C7 C8 C9 119.1(5) . . ?
C7 C8 C10 121.0(5) . . ?
C10 C8 C9 119.9(5) . . ?
O5 C9 O6 123.1(6) . . ?
O5 C9 C8 121.5(6) . . ?
O6 C9 C8 115.4(5) . . ?
C3 C10 C8 118.9(5) . . ?
C3 C10 H10 120.6 . . ?
C8 C10 H10 120.6 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O6 H6 O2 0.979(7) 1.59(4) 2.541(6) 162(11) 2
O7 H7A O5 0.980(7) 1.90(4) 2.833(9) 158(8) 2_746
O7 H7B O2 0.980(7) 2.15(2) 3.112(8) 169(9) 1_656
O8 H8A O1 0.978(7) 1.90(4) 2.785(6) 150(7) 2_656
O8 H8B O2 0.979(7) 2.25(5) 3.037(7) 137(6) 1_656
O8 H8B O5 0.979(7) 2.32(7) 3.025(8) 128(6) 2_646
N1 H1 O4 0.980(7) 2.32(6) 3.098(7) 136(7) 2_746


_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_e18adb3
_database_code_depnum_ccdc_archive 'CCDC 2097435'
loop_
_audit_author_name
_audit_author_address
'Mary Mahon'
;University of Bath
United Kingdom
;
_audit_update_record             
;
2021-07-19 deposited with the CCDC.	2021-12-20 downloaded from the CCDC.
;
_audit_creation_date             2018-08-24
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelxl_version_number           2014-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C10 H9.4 Cu N O7.2'
_chemical_formula_sum            'C10 H9.40 Cu N O7.20'
_chemical_formula_weight         322.32
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_usercomment     'Green-Blue Plate'
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'
Cu Cu 0.3201 1.2651 '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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   4.9056(5)
_cell_length_b                   9.7392(10)
_cell_length_c                   11.4649(14)
_cell_angle_alpha                90
_cell_angle_beta                 97.117(10)
_cell_angle_gamma                90
_cell_volume                     543.53(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1701
_cell_measurement_temperature    150.1(4)
_cell_measurement_theta_max      27.1300
_cell_measurement_theta_min      4.1640
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.044
_exptl_absorpt_correction_T_max  0.960
_exptl_absorpt_correction_T_min  0.690
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.969
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             326
_exptl_crystal_size_max          0.316
_exptl_crystal_size_mid          0.089
_exptl_crystal_size_min          0.019
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0541
_diffrn_reflns_av_unetI/netI     0.0916
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -3
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            2564
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.520
_diffrn_reflns_theta_min         3.582
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.1(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0734
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.879
_reflns_Friedel_fraction_full    0.990
_reflns_Friedel_fraction_max     0.984
_reflns_number_gt                2093
_reflns_number_total             2564
_reflns_special_details          
;
 _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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.564
_refine_diff_density_min         -1.000
_refine_diff_density_rms         0.109
_refine_ls_abs_structure_details 
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.01(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.953
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     198
_refine_ls_number_reflns         2564
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0481
_refine_ls_restrained_S_all      0.952
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0517P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0958
_refine_ls_wR_factor_ref         0.0989
_refine_special_details          
;
The asymmetric unit was seen to contain one full copper centre, 
one H-5-CMAI ligand, one full co-ordinated water ligand, and a 
water ligand with 20% occupancy, based on O8. 
The hydrogen atoms attached to O6, N1 and O7 were located, and 
subsequently refined at a distance of 0.98 Å away from their 
relevant parent atoms. The hydrogens attached to O8 were 
included at calculated positions, which seem to bear some 
credibility given that they are implicated in hydrogen 
bonding. 
The raw data for this analysis were were integrated to take 
account of crystal twinning, by virtue of a 180o rotation 
about the 1, 0, 0 direct axis. 
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.787(3)
 0.213(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H,H) groups
3. Restrained distances
 N1-H1
 0.98 with sigma of 0.005
 O7-H7B = O7-H7A = O6-H6
 0.98 with sigma of 0.005
4. Others
 Fixed Sof: O8(0.2) H8A(0.2) H8B(0.2)
 Fixed Uiso: H1(0.07)
5.a Rotating group:
 O8(H8A,H8B)
5.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B)
5.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C7(H7), C10(H10)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
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 0.6484(2) 0.16325(11) 0.25955(8) 0.0142(2) Uani 1 1 d . . . . .
O1 O 0.4282(15) 0.1956(6) 0.1078(5) 0.0207(19) Uani 1 1 d . . . . .
O2 O 0.4136(15) 0.3252(6) -0.0529(5) 0.0234(15) Uani 1 1 d . . . . .
O3 O 1.0957(14) 0.6165(5) 0.6050(5) 0.0155(14) Uani 1 1 d . . . . .
O4 O 0.7173(14) 0.7225(6) 0.6489(5) 0.0138(14) Uani 1 1 d . . . . .
O6 O 0.0221(14) 0.6875(7) 0.1407(5) 0.0214(18) Uani 1 1 d D . . . .
O5 O -0.0007(15) 0.8058(6) 0.3071(5) 0.0210(15) Uani 1 1 d . . . . .
O7 O 0.5462(14) -0.0325(6) 0.2503(5) 0.0205(15) Uani 1 1 d D . . . .
O8 O 0.970(9) 0.056(5) 0.121(3) 0.042(10) Uani 0.2 1 d . . P . .
H8A H 0.8908 -0.0128 0.0856 0.050 Uiso 0.2 1 d GR . P . .
H8B H 1.1109 0.0222 0.1618 0.050 Uiso 0.2 1 d GR . P . .
N1 N 0.8062(15) 0.3526(7) 0.2320(6) 0.0111(16) Uani 1 1 d D . . . .
C1 C 0.5207(19) 0.2920(9) 0.0480(8) 0.017(2) Uani 1 1 d . . . . .
C2 C 0.778(2) 0.3639(9) 0.1024(7) 0.0171(19) Uani 1 1 d . . . . .
H2A H 0.9373 0.3229 0.0734 0.021 Uiso 1 1 calc R . . . .
H2B H 0.7710 0.4600 0.0799 0.021 Uiso 1 1 calc R . . . .
C3 C 0.6914(19) 0.4608(8) 0.2932(7) 0.0121(18) Uani 1 1 d . . . . .
C4 C 0.8125(18) 0.4958(8) 0.4067(7) 0.0130(19) Uani 1 1 d . . . . .
H4 H 0.9666 0.4488 0.4414 0.016 Uiso 1 1 calc R . . . .
C5 C 0.6988(19) 0.6022(8) 0.4671(7) 0.0131(18) Uani 1 1 d . . . . .
C7 C 0.4705(17) 0.6717(14) 0.4165(6) 0.0162(17) Uani 1 1 d . . . . .
H7 H 0.3959 0.7412 0.4583 0.019 Uiso 1 1 calc R . . . .
C8 C 0.3484(19) 0.6395(9) 0.3029(7) 0.015(2) Uani 1 1 d . . . . .
C10 C 0.4614(19) 0.5341(8) 0.2420(7) 0.0151(19) Uani 1 1 d . . . . .
H10 H 0.3829 0.5121 0.1663 0.018 Uiso 1 1 calc R . . . .
C6 C 0.8431(18) 0.6500(12) 0.5840(6) 0.0133(18) Uani 1 1 d . . . . .
C9 C 0.1071(19) 0.7205(8) 0.2517(8) 0.0153(19) Uani 1 1 d . . . . .
H1 H 1.000(7) 0.346(13) 0.264(11) 0.070 Uiso 1 1 d D . . . .
H6 H -0.11(2) 0.753(10) 0.100(10) 0.07(4) Uiso 1 1 d D . . . .
H7A H 0.52(3) -0.068(11) 0.170(4) 0.05(4) Uiso 1 1 d D . . . .
H7B H 0.72(2) -0.067(16) 0.293(15) 0.13(8) Uiso 1 1 d 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
Cu1 O1 1.956(6) . ?
Cu1 O3 1.927(6) 2_746 ?
Cu1 O4 2.262(6) 2_646 ?
Cu1 O7 1.971(6) . ?
Cu1 O8 2.59(4) . ?
Cu1 N1 2.040(7) . ?
O1 C1 1.279(11) . ?
O2 C1 1.252(10) . ?
O3 Cu1 1.927(6) 2_756 ?
O3 C6 1.275(10) . ?
O4 Cu1 2.262(6) 2_656 ?
O4 C6 1.244(11) . ?
O6 C9 1.328(10) . ?
O6 H6 0.979(8) . ?
O5 C9 1.207(11) . ?
O7 H7A 0.980(8) . ?
O7 H7B 0.980(8) . ?
O8 H8A 0.8514 . ?
O8 H8B 0.8515 . ?
N1 C2 1.479(11) . ?
N1 C3 1.421(12) . ?
N1 H1 0.979(8) . ?
C1 C2 1.511(13) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.404(12) . ?
C3 C10 1.401(12) . ?
C4 H4 0.9300 . ?
C4 C5 1.400(11) . ?
C5 C7 1.374(13) . ?
C5 C6 1.509(11) . ?
C7 H7 0.9300 . ?
C7 C8 1.400(11) . ?
C8 C10 1.395(12) . ?
C8 C9 1.482(12) . ?
C10 H10 0.9300 . ?

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
O1 Cu1 O4 89.4(3) . 2_646 ?
O1 Cu1 O7 90.0(3) . . ?
O1 Cu1 O8 80.2(9) . . ?
O1 Cu1 N1 84.0(3) . . ?
O3 Cu1 O1 171.0(3) 2_746 . ?
O3 Cu1 O4 99.3(2) 2_746 2_646 ?
O3 Cu1 O7 87.2(2) 2_746 . ?
O3 Cu1 O8 90.8(9) 2_746 . ?
O3 Cu1 N1 96.7(3) 2_746 . ?
O4 Cu1 O8 164.7(9) 2_646 . ?
O7 Cu1 O4 93.5(2) . 2_646 ?
O7 Cu1 O8 75.4(10) . . ?
O7 Cu1 N1 164.8(3) . . ?
N1 Cu1 O4 100.4(3) . 2_646 ?
N1 Cu1 O8 89.8(10) . . ?
C1 O1 Cu1 113.7(6) . . ?
C6 O3 Cu1 127.8(6) . 2_756 ?
C6 O4 Cu1 127.9(6) . 2_656 ?
C9 O6 H6 114(7) . . ?
Cu1 O7 H7A 113(7) . . ?
Cu1 O7 H7B 96(10) . . ?
H7A O7 H7B 111(10) . . ?
Cu1 O8 H8A 109.3 . . ?
Cu1 O8 H8B 109.3 . . ?
H8A O8 H8B 104.5 . . ?
Cu1 N1 H1 105(8) . . ?
C2 N1 Cu1 103.5(5) . . ?
C2 N1 H1 110(8) . . ?
C3 N1 Cu1 114.4(6) . . ?
C3 N1 C2 116.6(7) . . ?
C3 N1 H1 107(8) . . ?
O1 C1 C2 117.0(8) . . ?
O2 C1 O1 123.3(8) . . ?
O2 C1 C2 119.7(8) . . ?
N1 C2 C1 110.4(7) . . ?
N1 C2 H2A 109.6 . . ?
N1 C2 H2B 109.6 . . ?
C1 C2 H2A 109.6 . . ?
C1 C2 H2B 109.6 . . ?
H2A C2 H2B 108.1 . . ?
C4 C3 N1 119.3(8) . . ?
C10 C3 N1 121.2(7) . . ?
C10 C3 C4 119.4(8) . . ?
C3 C4 H4 120.4 . . ?
C5 C4 C3 119.3(8) . . ?
C5 C4 H4 120.4 . . ?
C4 C5 C6 119.7(8) . . ?
C7 C5 C4 120.6(8) . . ?
C7 C5 C6 119.4(8) . . ?
C5 C7 H7 119.5 . . ?
C5 C7 C8 121.0(9) . . ?
C8 C7 H7 119.5 . . ?
C7 C8 C9 118.6(8) . . ?
C10 C8 C7 118.7(8) . . ?
C10 C8 C9 122.8(8) . . ?
C3 C10 H10 119.5 . . ?
C8 C10 C3 121.0(7) . . ?
C8 C10 H10 119.5 . . ?
O3 C6 C5 115.3(8) . . ?
O4 C6 O3 125.1(8) . . ?
O4 C6 C5 119.6(8) . . ?
O6 C9 C8 113.0(8) . . ?
O5 C9 O6 124.4(9) . . ?
O5 C9 C8 122.6(8) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O8 H8A O2 0.85 2.17 2.97(5) 156.5 2_645
O8 H8B O7 0.85 2.31 3.14(4) 166.8 1_655
C2 H2A O8 0.97 2.66 3.14(4) 111.3 .
N1 H1 O4 0.979(8) 2.00(8) 2.854(9) 144(10) 2_746
O6 H6 O2 0.979(8) 1.68(5) 2.617(9) 158(13) 2
O7 H7A O2 0.980(8) 1.76(5) 2.682(9) 156(10) 2_645
O7 H7B O5 0.980(8) 1.85(9) 2.736(9) 149(15) 1_645


_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.787(3) 1418 2814 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000
0.0000 1.0000
2 0.213(3) 0 2814 nmt 1.0006 0.0003 -0.0004 -0.0009 -1.0001 -0.0005 -0.5944
-0.0000 -1.0004

_twin_special_details            
;
Component 2 rotated by -179.9814° 
 around [0.96 -0.00 -0.28] (reciprocal) or [1.00 0.00 -0.00] (direct)
;
####################################################################### 
# 
# 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_e18adb10
_database_code_depnum_ccdc_archive 'CCDC 2097437'
loop_
_audit_author_name
_audit_author_address
'Mary Mahon'
;University of Bath
United Kingdom
;
_audit_update_record             
;
2021-07-19 deposited with the CCDC.	2021-12-20 downloaded from the CCDC.
;
_audit_creation_date             2019-01-11
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelxl_version_number           2014-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C10 H11 N O9 Zn2, H2 O, 2(O)'
_chemical_formula_sum            'C10 H17 N O12 Zn2'
_chemical_formula_weight         473.98
_chemical_melting_point          ?
_chemical_oxdiff_usercomment     'Very light tan block'
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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
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                   7.4213(3)
_cell_length_b                   19.3205(6)
_cell_length_c                   10.8081(4)
_cell_angle_alpha                90
_cell_angle_beta                 96.871(3)
_cell_angle_gamma                90
_cell_volume                     1538.57(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5772
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      29.5550
_cell_measurement_theta_min      4.0880
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.186
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81256
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light tan'
_exptl_crystal_colour_primary    ?
_exptl_crystal_density_diffrn    2.046
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.277
_exptl_crystal_size_mid          0.239
_exptl_crystal_size_min          0.105
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_unetI/netI     0.0389
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12808
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.479
_diffrn_reflns_theta_min         3.332
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0734
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3070
_reflns_number_total             3507
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         1.599
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.103
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     278
_refine_ls_number_reflns         3507
_refine_ls_number_restraints     40
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.0323
_refine_ls_restrained_S_all      1.079
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0315P)²+2.3458P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0774
_refine_ls_wR_factor_ref         0.0808
_refine_special_details          
;
The asymmetric unit contains 2 cadmium centres, one 5-CMAI ligand, one 
hydroxide ion, two coordinated water ligands (one to each of the cadmiums) 
and three guest water molecules. Only one of the latter is ordered 
(based on O10); those based on O11 and O12 are have been modelled, 
with ADP restraints, to take account of disorder over 5 regions in 
a 25:65:20:80:10 ratio. This disorder is not altogether unsurprising 
as, in the gross structure (covalently bonded sheets, linked by 
hydrogen bonding [Table 6]), the fragment waters reside in are 
channels along the 1,0,1 direction. 
Hydrogen atoms were not included for the disordered waters, 
but in the ordered portion of the structure, oxygen and nitrogen 
bound hydrogens were located and refined at a distance of 
0.98 Å from the relevant parent atom. 
The residual electron density maximum is located at 1.64 Å 
from O2, and is chemically insignificant. The spurious nature 
of this peak may arise from the fact that there is evidence of 
some twinning (136o about the -0.2, 0.95, 0.21 vector) in the 
raw data frames.  However, the level of twinning ( < 5%) did 
not merit retension in the final refinement. 

;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All H(H,H,H) groups, All O(H) groups, All O(H,H,H) groups
2. Restrained distances
 N1-H1
 0.98 with sigma of 0.005
 O9-H9
 0.98 with sigma of 0.005
 O8-H8A = O8-H8B = O10-H10B
 0.98 with sigma of 0.005
 O10-H10A
 0.98 with sigma of 0.005
 O7-H7A = O7-H7B
 0.98 with sigma of 0.005
 H7B-H7A
 1.55 with sigma of 0.009
 H8A-H8B
 1.55 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
O11A \\sim O12 \\sim O11 \\sim O12A \\sim O11B: within 2A with sigma of 0.02
and sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: O11A(0.65) O12(0.8) O11(0.25) O12A(0.1) O11B(0.2)
5.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B)
5.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C7(H7), C10(H10)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
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 0.75518(4) 0.56904(2) 0.30008(3) 0.01056(10) Uani 1 1 d . . . . .
Zn2 Zn 1.03115(4) 0.44993(2) 0.39210(3) 0.01116(10) Uani 1 1 d . . . . .
O1 O 1.0356(3) 0.54652(10) 0.28273(19) 0.0133(4) Uani 1 1 d . . . . .
O2 O 1.2255(3) 0.52787(12) 0.1418(2) 0.0192(5) Uani 1 1 d . . . . .
O3 O 0.5292(3) 0.85648(10) 0.0296(2) 0.0174(5) Uani 1 1 d . . . . .
O4 O 0.2891(3) 0.83643(10) -0.1122(2) 0.0159(5) Uani 1 1 d . . . . .
O5 O 0.1301(3) 0.59347(10) -0.23620(19) 0.0150(4) Uani 1 1 d . . . . .
O6 O 0.3508(3) 0.51404(10) -0.1963(2) 0.0155(4) Uani 1 1 d . . . . .
O7 O 0.4797(3) 0.60229(13) 0.2909(2) 0.0248(5) Uani 1 1 d D . . . .
H7A H 0.446(5) 0.6493(6) 0.264(3) 0.037 Uiso 1 1 d DR . . . .
H7B H 0.392(4) 0.5720(12) 0.243(3) 0.037 Uiso 1 1 d DR . . . .
H10A H 0.573(6) 0.388(2) 0.5491(13) 0.037 Uiso 1 1 d DR . . . .
O8 O 1.2617(3) 0.41708(12) 0.3098(2) 0.0200(5) Uani 1 1 d D . . . .
O9 O 0.8194(3) 0.50882(10) 0.45396(18) 0.0116(4) Uani 1 1 d D . . . .
H9 H 0.722(3) 0.4768(13) 0.468(3) 0.017 Uiso 1 1 d DR . . . .
N1 N 0.8115(3) 0.62438(12) 0.1302(2) 0.0113(5) Uani 1 1 d D . . . .
H1 H 0.878(4) 0.6654(10) 0.164(3) 0.011(8) Uiso 1 1 d D . . . .
H8A H 1.296(3) 0.4544(12) 0.256(2) 0.017 Uiso 1 1 d DR . . . .
H8B H 1.375(2) 0.4047(14) 0.361(2) 0.017 Uiso 1 1 d DR . . . .
H10B H 0.7181(15) 0.3651(17) 0.462(3) 0.017 Uiso 1 1 d DR . . . .
C1 C 1.0802(4) 0.55012(14) 0.1730(3) 0.0134(6) Uani 1 1 d . . . . .
C2 C 0.9447(4) 0.58243(16) 0.0731(3) 0.0150(6) Uani 1 1 d . . . . .
H2A H 1.0084 0.6114 0.0192 0.018 Uiso 1 1 calc R . . . .
H2B H 0.8824 0.5462 0.0226 0.018 Uiso 1 1 calc R . . . .
C3 C 0.6587(4) 0.64699(15) 0.0457(3) 0.0117(6) Uani 1 1 d . . . . .
C4 C 0.6152(4) 0.71710(14) 0.0428(3) 0.0124(6) Uani 1 1 d . . . . .
H4 H 0.6857 0.7481 0.0936 0.015 Uiso 1 1 calc R . . . .
C5 C 0.4665(4) 0.74083(14) -0.0361(3) 0.0126(6) Uani 1 1 d . . . . .
C6 C 0.4249(4) 0.81725(14) -0.0402(3) 0.0126(6) Uani 1 1 d . . . . .
C7 C 0.3581(4) 0.69487(15) -0.1100(3) 0.0132(6) Uani 1 1 d . . . . .
H7 H 0.2581 0.7109 -0.1622 0.016 Uiso 1 1 calc R . . . .
C8 C 0.3996(4) 0.62439(14) -0.1059(3) 0.0111(6) Uani 1 1 d . . . . .
C9 C 0.2842(4) 0.57321(14) -0.1860(3) 0.0123(6) Uani 1 1 d . . . . .
C10 C 0.5506(4) 0.60050(14) -0.0285(3) 0.0118(6) Uani 1 1 d . . . . .
H10 H 0.5792 0.5536 -0.0265 0.014 Uiso 1 1 calc R . . . .
O11A O 0.4008(11) 0.7655(3) 0.2912(9) 0.052(2) Uani 0.65 1 d . U P A 1
O12 O 0.0656(5) 0.74472(17) 0.1175(5) 0.0610(14) Uani 0.8 1 d . U P B 1
O11 O 0.407(3) 0.8016(10) 0.318(2) 0.076(5) Uani 0.25 1 d . U P C 2
O12A O 0.233(5) 0.6954(16) 0.203(4) 0.059(6) Uani 0.1 1 d . U P D 2
O11B O 0.374(4) 0.7406(12) 0.272(3) 0.055(5) Uani 0.2 1 d . U P E 5
O10 O 0.5909(3) 0.37822(15) 0.4625(2) 0.0323(6) Uani 1 1 d 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
Zn1 O1 2.156(2) . ?
Zn1 O4 2.059(2) 4_676 ?
Zn1 O6 2.060(2) 3_665 ?
Zn1 O7 2.134(2) . ?
Zn1 O9 2.0390(19) . ?
Zn1 N1 2.208(2) . ?
Zn2 Zn2 3.1074(7) 3_766 ?
Zn2 O1 2.211(2) . ?
Zn2 O3 2.066(2) 2_645 ?
Zn2 O5 2.119(2) 3_665 ?
Zn2 O8 2.118(2) . ?
Zn2 O9 2.0475(19) 3_766 ?
Zn2 O9 2.113(2) . ?
O1 C1 1.271(4) . ?
O2 C1 1.244(4) . ?
O3 Zn2 2.066(2) 2_655 ?
O3 C6 1.266(3) . ?
O4 Zn1 2.059(2) 4_575 ?
O4 C6 1.253(3) . ?
O5 Zn2 2.119(2) 3_665 ?
O5 C9 1.267(3) . ?
O6 Zn1 2.060(2) 3_665 ?
O6 C9 1.256(3) . ?
O7 H7A 0.977(5) . ?
O7 H7B 0.977(5) . ?
O8 H8A 0.980(5) . ?
O8 H8B 0.978(5) . ?
O9 Zn2 2.0475(19) 3_766 ?
O9 H9 0.977(5) . ?
N1 H1 0.978(5) . ?
N1 C2 1.469(4) . ?
N1 C3 1.436(3) . ?
C1 C2 1.519(4) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.392(4) . ?
C3 C10 1.393(4) . ?
C4 H4 0.9300 . ?
C4 C5 1.389(4) . ?
C5 C6 1.508(4) . ?
C5 C7 1.386(4) . ?
C7 H7 0.9300 . ?
C7 C8 1.395(4) . ?
C8 C9 1.511(4) . ?
C8 C10 1.395(4) . ?
C10 H10 0.9300 . ?
O10 H10A 0.979(5) . ?
O10 H10B 0.978(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
O1 Zn1 N1 75.20(8) . . ?
O4 Zn1 O1 98.79(8) 4_676 . ?
O4 Zn1 O6 163.67(8) 4_676 3_665 ?
O4 Zn1 O7 79.53(9) 4_676 . ?
O4 Zn1 N1 85.91(9) 4_676 . ?
O6 Zn1 O1 96.03(8) 3_665 . ?
O6 Zn1 O7 84.72(9) 3_665 . ?
O6 Zn1 N1 91.28(9) 3_665 . ?
O7 Zn1 O1 170.40(9) . . ?
O7 Zn1 N1 95.22(9) . . ?
O9 Zn1 O1 79.74(8) . . ?
O9 Zn1 O4 97.28(8) . 4_676 ?
O9 Zn1 O6 92.08(8) . 3_665 ?
O9 Zn1 O7 109.82(9) . . ?
O9 Zn1 N1 154.93(9) . . ?
O1 Zn2 Zn2 83.61(5) . 3_766 ?
O3 Zn2 Zn2 100.22(7) 2_645 3_766 ?
O3 Zn2 O1 167.01(8) 2_645 . ?
O3 Zn2 O5 81.41(8) 2_645 3_665 ?
O3 Zn2 O8 97.82(9) 2_645 . ?
O3 Zn2 O9 97.75(8) 2_645 . ?
O5 Zn2 Zn2 136.26(6) 3_665 3_766 ?
O5 Zn2 O1 87.25(8) 3_665 . ?
O8 Zn2 Zn2 134.59(6) . 3_766 ?
O8 Zn2 O1 87.93(8) . . ?
O8 Zn2 O5 87.44(8) . 3_665 ?
O9 Zn2 Zn2 42.48(6) 3_766 3_766 ?
O9 Zn2 Zn2 40.88(5) . 3_766 ?
O9 Zn2 O1 93.70(8) 3_766 . ?
O9 Zn2 O1 76.93(7) . . ?
O9 Zn2 O3 97.48(8) 3_766 2_645 ?
O9 Zn2 O5 178.21(8) 3_766 3_665 ?
O9 Zn2 O5 95.39(8) . 3_665 ?
O9 Zn2 O8 94.11(8) 3_766 . ?
O9 Zn2 O8 164.42(8) . . ?
O9 Zn2 O9 83.36(8) 3_766 . ?
Zn1 O1 Zn2 92.73(8) . . ?
C1 O1 Zn1 115.60(18) . . ?
C1 O1 Zn2 124.55(18) . . ?
C6 O3 Zn2 128.33(19) . 2_655 ?
C6 O4 Zn1 126.38(19) . 4_575 ?
C9 O5 Zn2 127.79(19) . 3_665 ?
C9 O6 Zn1 128.97(19) . 3_665 ?
Zn1 O7 H7A 120(2) . . ?
Zn1 O7 H7B 115(2) . . ?
H7A O7 H7B 105.7(10) . . ?
Zn2 O8 H8A 108.0(18) . . ?
Zn2 O8 H8B 121.3(18) . . ?
H8A O8 H8B 104.5(7) . . ?
Zn1 O9 Zn2 119.45(9) . 3_766 ?
Zn1 O9 Zn2 99.17(9) . . ?
Zn1 O9 H9 112(2) . . ?
Zn2 O9 Zn2 96.64(8) 3_766 . ?
Zn2 O9 H9 117(2) 3_766 . ?
Zn2 O9 H9 108(2) . . ?
Zn1 N1 H1 102.8(19) . . ?
C2 N1 Zn1 106.60(17) . . ?
C2 N1 H1 105.6(19) . . ?
C3 N1 Zn1 117.52(18) . . ?
C3 N1 H1 108.1(18) . . ?
C3 N1 C2 114.9(2) . . ?
O1 C1 C2 117.5(3) . . ?
O2 C1 O1 124.4(3) . . ?
O2 C1 C2 118.1(3) . . ?
N1 C2 C1 110.5(2) . . ?
N1 C2 H2A 109.6 . . ?
N1 C2 H2B 109.6 . . ?
C1 C2 H2A 109.6 . . ?
C1 C2 H2B 109.6 . . ?
H2A C2 H2B 108.1 . . ?
C4 C3 N1 118.3(2) . . ?
C4 C3 C10 119.9(3) . . ?
C10 C3 N1 121.8(3) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 C3 120.0(3) . . ?
C5 C4 H4 120.0 . . ?
C4 C5 C6 119.1(3) . . ?
C7 C5 C4 120.4(3) . . ?
C7 C5 C6 120.5(3) . . ?
O3 C6 C5 117.4(2) . . ?
O4 C6 O3 125.6(3) . . ?
O4 C6 C5 117.0(3) . . ?
C5 C7 H7 120.1 . . ?
C5 C7 C8 119.7(3) . . ?
C8 C7 H7 120.1 . . ?
C7 C8 C9 120.8(3) . . ?
C10 C8 C7 120.0(3) . . ?
C10 C8 C9 119.1(2) . . ?
O5 C9 C8 117.6(2) . . ?
O6 C9 O5 126.0(3) . . ?
O6 C9 C8 116.4(2) . . ?
C3 C10 C8 119.9(3) . . ?
C3 C10 H10 120.1 . . ?
C8 C10 H10 120.1 . . ?
H10A O10 H10B 107(3) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O7 H7A O12A 0.977(5) 1.87(4) 2.66(4) 136(3) .
O7 H7A O11B 0.977(5) 1.85(3) 2.79(2) 160(4) .
O7 H7B O2 0.977(5) 1.767(8) 2.737(3) 172(3) 1_455
O10 H10A O7 0.979(5) 1.829(8) 2.803(4) 173(4) 3_666
O9 H9 O10 0.977(5) 2.136(16) 3.048(3) 155(3) .
N1 H1 O12 0.978(5) 2.17(2) 3.007(4) 143(3) 1_655
O8 H8A O2 0.980(5) 1.910(13) 2.799(3) 149(2) .
O8 H8B O10 0.978(5) 1.902(6) 2.879(3) 178(2) 1_655
O10 H10B O3 0.978(5) 1.874(9) 2.842(3) 170(3) 2_645


_olex2_submission_special_instructions 'No special instructions were received'
#===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_s19adb23
_database_code_depnum_ccdc_archive 'CCDC 2097432'
loop_
_audit_author_name
_audit_author_address
'Mary Mahon'
;University of Bath
United Kingdom
;
_audit_update_record             
;
2021-07-19 deposited with the CCDC.	2021-12-20 downloaded from the CCDC.
;
_audit_creation_date             2019-11-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C46.75 H59.25 Cd6 N6.25 O36, 0.6(C3 H7 N O)'
_chemical_formula_sum            'C51.25 H105.75 Cd6 N7.75 O55.50'
_chemical_formula_weight         2393.08
_chemical_absolute_configuration syn
_chemical_melting_point          ?
_chemical_oxdiff_usercomment     'Colourless Shard'
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'
Cd Cd 0.1185 4.6533 '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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   14.10810(10)
_cell_length_b                   14.3068(2)
_cell_length_c                   23.1617(3)
_cell_angle_alpha                90
_cell_angle_beta                 90.9450(10)
_cell_angle_gamma                90
_cell_volume                     4674.36(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    23833
_cell_measurement_temperature    220.00(10)
_cell_measurement_theta_max      72.9320
_cell_measurement_theta_min      3.6940
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    11.633
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64233
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.700
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2399
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.085
_exptl_crystal_size_min          0.031
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            66896
_diffrn_reflns_point_group_measured_fraction_full 0.920
_diffrn_reflns_point_group_measured_fraction_max 0.910
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.074
_diffrn_reflns_theta_min         3.133
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      220.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1150
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.752
_reflns_Friedel_fraction_full    0.834
_reflns_Friedel_fraction_max     0.816
_reflns_number_gt                16197
_reflns_number_total             17026
_reflns_special_details          
;
The compound s19adb23 crystallises in a monoclinic space group P21, and was 
something of a challenge to solve and refine. Inherent diffraction weaknesses, 
most likely related to pseudosymmetry involving the cadmium centres and their 
dominance in the reflection intensities, automatically predicted solution in 
space group C2, along with a reduction in the size of the asymmetric unit of 
50%, but concomitant loss of guest solvent and resolution of ligated DMF. 
Ultimately, examination of calculated diffraction nets, from the raw data 
frames led to selection of the correct space group symmetry.

The asymmetric unit contains 6 cadmium centres, 4 5-CMAI linkers, 9 full 
water ligands, 2 partial waters, 1 full DMF ligand and 2 partial DMF ligands. 
There is also a substantial amount of guest solvent, of which only 0.6 DMF 
molecules were resolved fully, with an addition 18 water molecules and 0.9 
DMF molecules removed using a solvent mask. The structure builds up into a 
three-dimensional lattice with convoluted cavities and channels in which 
the guest solvent resides. 

 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         3.787
_refine_diff_density_min         -1.506
_refine_diff_density_rms         0.180
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.419(13)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1020
_refine_ls_number_reflns         17026
_refine_ls_number_restraints     219
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0626
_refine_ls_restrained_S_all      1.008
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1035P)²+25.2960P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1711
_refine_ls_wR_factor_ref         0.1735
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.581(13)
 0.419(13)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
3. Restrained distances
 H27A-Cd1
 2.8 with sigma of 0.04
 H27B-Cd1
 2.8 with sigma of 0.04
 H26B-Cd1
 2.8 with sigma of 0.04
 H26A-Cd1
 2.8 with sigma of 0.04
 H28B-Cd1
 2.8 with sigma of 0.04
 H28A-Cd1
 2.8 with sigma of 0.04
 H31B-Cd2
 2.8 with sigma of 0.04
 H31A-Cd2
 2.8 with sigma of 0.04
 H32B-Cd2
 2.8 with sigma of 0.04
 H32A-Cd2
 2.8 with sigma of 0.04
 H30B-Cd2
 2.8 with sigma of 0.04
 H30A-Cd2
 2.8 with sigma of 0.04
 H35B-Cd3
 2.8 with sigma of 0.04
 H35A-Cd3
 2.8 with sigma of 0.04
 H34B-Cd3
 2.8 with sigma of 0.04
 H34A-Cd3
 2.8 with sigma of 0.04
 H38B-Cd4
 2.8 with sigma of 0.04
 H37B-Cd4
 2.8 with sigma of 0.04
 H37A-Cd4
 2.8 with sigma of 0.04
 H36A-Cd4
 2.8 with sigma of 0.04
 H36B-Cd4
 2.8 with sigma of 0.04
 H38A-Cd4
 2.8 with sigma of 0.04
 O26-H26B = O26-H26A = O27-H27B = O27-H27A = O28-H28B = O28-H28A = O32-H32A =
 O32-H32B = O31-H31A = O31-H31B = O30-H30A = O30-H30B = O34-H34B = O34-H34A =
 O35-H35B = O35-H35A = O36-H36A = O36-H36B = O38-H38A = O38-H38B = O37-H37A =
 O37-H37B
 0.98 with sigma of 0.005
 H36A-H36B \\sim H37B-H37A \\sim H35B-H35A \\sim H34A-H34B \\sim H38B-H38A
\\sim H30A-H30B \\sim H31A-
 H31B \\sim H32B-H32A \\sim H26B-H26A \\sim H27A-H27B \\sim H28A-H28B
 with sigma of 0.005
4. Uiso/Uaniso restraints and constraints
O29 \\sim N6 \\sim C44 \\sim C45 \\sim C46 \\sim O30: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.005
C42 \\sim O25 \\sim N5 \\sim C41 \\sim C43 \\sim O26: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.005
O33 \\sim N7 \\sim C47 \\sim C48 \\sim C49: within 2A with sigma of 0.05 and
sigma for terminal atoms of 0.01
O40 \\sim N9 \\sim C53 \\sim C54 \\sim C55: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.005
5. Others
 Fixed Sof: C42(0.7) H42A(0.7) H42B(0.7) H42C(0.7) O25(0.7) O29(0.55) N5(0.7)
 N6(0.55) C41(0.7) H41(0.7) C43(0.7) H43A(0.7) H43B(0.7) H43C(0.7) C44(0.55)
 H44(0.55) C45(0.55) H45A(0.55) H45B(0.55) H45C(0.55) C46(0.55) H46A(0.55)
 H46B(0.55) H46C(0.55) O26(0.3) H26A(0.3) H26B(0.3) O30(0.45) H30A(0.45)
 H30B(0.45) O40(0.6) N9(0.6) C53(0.6) H53(0.6) C54(0.6) H54A(0.6) H54B(0.6)
 H54C(0.6) C55(0.6) H55A(0.6) H55B(0.6) H55C(0.6)
 Fixed Y: Cd1(0.82707)
6.a Ternary CH refined with riding coordinates:
 N1(H1), N2(H2), N3(H3), N4(H4)
6.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C12(H12A,H12B), C22(H22A,H22B), C32(H32C,H32D)
6.c Aromatic/amide H refined with riding coordinates:
 C4(H4A), C7(H7), C10(H10), C14(H14), C17(H17), C20(H20), C24(H24), C27(H27),
 C30(H30), C34(H34), C37(H37), C40(H40), C47(H47), C41(H41), C44(H44), C53(H53)
6.d Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C43(H43A,H43B,
 H43C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C54(H54A,H54B,H54C), C55(H55A,
 H55B,H55C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.84753(6) 0.827070 0.73210(3) 0.0295(2) Uani 1 1 d D . . . .
Cd2 Cd 0.69232(7) 0.48545(11) 0.76425(4) 0.0401(3) Uani 1 1 d D . . . .
Cd3 Cd 0.33899(6) 0.33658(9) 0.73930(4) 0.0373(3) Uani 1 1 d D . . . .
Cd4 Cd 0.20175(6) -0.01932(9) 0.76619(4) 0.0318(2) Uani 1 1 d D . . . .
Cd5 Cd 0.74483(4) 0.39091(10) 0.49987(2) 0.01482(16) Uani 1 1 d . . . . .
Cd6 Cd 0.24837(4) 0.38914(10) 0.99897(2) 0.01537(16) Uani 1 1 d . . . . .
O1 O 0.9995(6) 0.8816(8) 0.7449(3) 0.033(2) Uani 1 1 d . . . . .
O2 O 1.1405(6) 0.8349(8) 0.7797(5) 0.042(2) Uani 1 1 d . . . . .
O3 O 0.8221(6) 0.4642(6) 0.5731(3) 0.0292(18) Uani 1 1 d . . . . .
O4 O 0.8899(7) 0.5042(8) 0.4920(4) 0.045(3) Uani 1 1 d . . . . .
O5 O 1.1336(7) 0.7612(7) 0.4940(3) 0.034(2) Uani 1 1 d . . . . .
O6 O 1.1865(6) 0.8133(6) 0.5771(3) 0.0268(17) Uani 1 1 d . . . . .
O7 O 0.7467(6) 0.6311(7) 0.7463(4) 0.035(2) Uani 1 1 d . . . . .
O8 O 0.6996(7) 0.7751(7) 0.7174(4) 0.041(2) Uani 1 1 d . . . . .
O9 O 0.3296(6) 0.4484(8) 0.9189(4) 0.040(2) Uani 1 1 d . . . . .
O10 O 0.3728(8) 0.5097(9) 1.0034(4) 0.045(3) Uani 1 1 d . . . . .
O11 O 0.6395(9) 0.7496(11) 1.0094(5) 0.058(4) Uani 1 1 d . . . . .
O12 O 0.6716(6) 0.8144(6) 0.9262(4) 0.0331(19) Uani 1 1 d . . . . .
O13 O 0.4909(6) 0.3896(9) 0.7557(4) 0.039(2) Uani 1 1 d . . . . .
O14 O 0.6356(7) 0.3371(10) 0.7787(5) 0.048(3) Uani 1 1 d . . . . .
O15 O 0.3108(6) -0.0234(7) 0.5816(3) 0.037(2) Uani 1 1 d . . . . .
O16 O 0.3652(7) 0.0251(8) 0.4980(4) 0.037(2) Uani 1 1 d . . . . .
O17 O 0.6136(6) 0.2785(7) 0.4992(3) 0.029(2) Uani 1 1 d . . . . .
O18 O 0.6681(6) 0.3287(8) 0.5833(3) 0.040(2) Uani 1 1 d . . . . .
O19 O 0.2464(6) 0.1329(8) 0.7546(4) 0.034(2) Uani 1 1 d . . . . .
O20 O 0.1985(8) 0.2664(8) 0.7239(4) 0.044(2) Uani 1 1 d . . . . .
O21 O -0.1664(6) -0.0570(7) 0.9198(4) 0.035(2) Uani 1 1 d . . . . .
O22 O -0.1375(9) 0.0093(10) 0.9995(5) 0.055(3) Uani 1 1 d . . . . .
O23 O 0.1242(8) 0.2625(9) 1.0041(4) 0.048(3) Uani 1 1 d . . . . .
O24 O 0.1676(6) 0.3160(7) 0.9220(4) 0.038(2) Uani 1 1 d . . . . .
O27 O 0.8397(9) 0.8020(7) 0.8314(4) 0.046(3) Uani 1 1 d D . . . .
H27A H 0.794(6) 0.751(6) 0.837(3) 0.068 Uiso 1 1 d DR . . . .
H27B H 0.9047(19) 0.792(9) 0.846(3) 0.068 Uiso 1 1 d DR . . . .
O28 O 0.8540(7) 0.8719(8) 0.6377(4) 0.043(2) Uani 1 1 d D . . . .
H28A H 0.912(4) 0.907(8) 0.629(3) 0.065 Uiso 1 1 d DR . . . .
H28B H 0.794(3) 0.898(9) 0.623(3) 0.065 Uiso 1 1 d DR . . . .
O31 O 0.8348(10) 0.4241(17) 0.7511(7) 0.112(8) Uani 1 1 d D . . . .
H31A H 0.857(7) 0.423(16) 0.7112(15) 0.168 Uiso 1 1 d DR . . . .
H31B H 0.882(5) 0.436(14) 0.782(4) 0.168 Uiso 1 1 d DR . . . .
O32 O 0.6576(9) 0.4737(10) 0.6681(5) 0.058(3) Uani 1 1 d D . . . .
H32A H 0.655(11) 0.4090(19) 0.654(3) 0.087 Uiso 1 1 d DR . . . .
H32B H 0.692(8) 0.519(6) 0.644(2) 0.087 Uiso 1 1 d DR . . . .
O33 O 0.3451(10) 0.3814(12) 0.6456(5) 0.071(4) Uani 1 1 d . U . . .
O34 O 0.2653(9) 0.4627(8) 0.7550(6) 0.057(3) Uani 1 1 d D . . . .
H34A H 0.227(10) 0.470(6) 0.790(4) 0.086 Uiso 1 1 d DR . . . .
H34B H 0.266(11) 0.515(5) 0.728(4) 0.086 Uiso 1 1 d DR . . . .
O35 O 0.3357(8) 0.3051(9) 0.8377(4) 0.047(3) Uani 1 1 d D . . . .
H35A H 0.287(6) 0.260(6) 0.849(3) 0.071 Uiso 1 1 d DR . . . .
H35B H 0.343(9) 0.362(3) 0.861(2) 0.071 Uiso 1 1 d DR . . . .
O36 O 0.1702(8) -0.0190(10) 0.6665(5) 0.053(3) Uani 1 1 d D . . . .
H36A H 0.197(8) -0.078(5) 0.652(3) 0.080 Uiso 1 1 d DR . . . .
H36B H 0.102(2) -0.008(9) 0.660(3) 0.080 Uiso 1 1 d DR . . . .
O37 O 0.3403(8) -0.0885(11) 0.7432(6) 0.071(4) Uani 1 1 d D . . . .
H37A H 0.332(5) -0.146(5) 0.721(5) 0.107 Uiso 1 1 d DR . . . .
H37B H 0.386(5) -0.089(9) 0.776(3) 0.107 Uiso 1 1 d DR . . . .
O38 O 0.2534(9) -0.0153(8) 0.8611(4) 0.053(3) Uani 1 1 d D . . . .
H38A H 0.220(7) 0.036(6) 0.880(3) 0.079 Uiso 1 1 d DR . . . .
H38B H 0.3229(11) -0.013(10) 0.862(3) 0.079 Uiso 1 1 d DR . . . .
N1 N 0.9515(7) 0.6945(7) 0.7237(4) 0.0206(19) Uani 1 1 d . . . . .
H1 H 0.919327 0.640273 0.740273 0.025 Uiso 1 1 calc R . . . .
N2 N 0.5610(9) 0.5837(9) 0.7751(5) 0.037(3) Uani 1 1 d . . . . .
H2 H 0.505581 0.551669 0.758432 0.044 Uiso 1 1 calc R . . . .
N3 N 0.4427(7) 0.2034(7) 0.7319(4) 0.026(2) Uani 1 1 d . . . . .
H3 H 0.410351 0.149325 0.748571 0.032 Uiso 1 1 calc R . . . .
N4 N 0.0637(8) 0.0759(9) 0.7738(5) 0.036(3) Uani 1 1 d . . . . .
H4 H 0.010611 0.041036 0.756489 0.043 Uiso 1 1 calc R . . . .
N7 N 0.3310(13) 0.4889(14) 0.5720(9) 0.084(4) Uani 1 1 d . U . . .
C1 C 1.0589(11) 0.8178(13) 0.7642(6) 0.048(4) Uani 1 1 d . . . . .
C2 C 1.0329(12) 0.7152(10) 0.7600(5) 0.036(3) Uani 1 1 d . . . . .
H2A H 1.086978 0.681223 0.745495 0.044 Uiso 1 1 calc R . . . .
H2B H 1.020816 0.692191 0.798616 0.044 Uiso 1 1 calc R . . . .
C3 C 0.9746(8) 0.6716(9) 0.6639(5) 0.026(2) Uani 1 1 d . . . . .
C4 C 0.9197(8) 0.6026(9) 0.6346(4) 0.023(2) Uani 1 1 d . . . . .
H4A H 0.871699 0.570688 0.653295 0.028 Uiso 1 1 calc R . . . .
C5 C 0.9398(8) 0.5841(8) 0.5771(5) 0.026(2) Uani 1 1 d . . . . .
C6 C 0.8804(8) 0.5126(8) 0.5454(5) 0.024(2) Uani 1 1 d . . . . .
C7 C 1.0088(7) 0.6383(7) 0.5482(4) 0.0183(19) Uani 1 1 d . . . . .
H7 H 1.019094 0.629378 0.508991 0.022 Uiso 1 1 calc R . . . .
C8 C 1.0581(7) 0.7010(8) 0.5773(4) 0.023(2) Uani 1 1 d . . . . .
C9 C 1.1285(8) 0.7645(7) 0.5468(5) 0.020(2) Uani 1 1 d . . . . .
C10 C 1.0434(8) 0.7217(7) 0.6346(4) 0.022(2) Uani 1 1 d . . . . .
H10 H 1.078695 0.767954 0.653186 0.026 Uiso 1 1 calc R . . . .
C11 C 0.6854(10) 0.6924(10) 0.7353(5) 0.033(3) Uani 1 1 d . . . . .
C12 C 0.5803(10) 0.6662(10) 0.7389(6) 0.040(3) Uani 1 1 d . . . . .
H12A H 0.545851 0.719192 0.754094 0.048 Uiso 1 1 calc R . . . .
H12B H 0.556036 0.654284 0.700143 0.048 Uiso 1 1 calc R . . . .
C13 C 0.5427(9) 0.6007(9) 0.8335(5) 0.030(3) Uani 1 1 d . . . . .
C14 C 0.4722(9) 0.5477(10) 0.8610(5) 0.033(3) Uani 1 1 d . . . . .
H14 H 0.436039 0.505201 0.839758 0.039 Uiso 1 1 calc R . . . .
C15 C 0.4564(8) 0.5589(8) 0.9202(4) 0.023(2) Uani 1 1 d . . . . .
C16 C 0.3809(9) 0.5034(8) 0.9488(5) 0.029(2) Uani 1 1 d . . . . .
C17 C 0.5105(8) 0.6290(10) 0.9510(5) 0.031(3) Uani 1 1 d . . . . .
H17 H 0.499036 0.640069 0.989827 0.037 Uiso 1 1 calc R . . . .
C18 C 0.5777(8) 0.6786(9) 0.9237(5) 0.026(2) Uani 1 1 d . . . . .
C19 C 0.6336(8) 0.7524(10) 0.9531(5) 0.030(3) Uani 1 1 d . . . . .
C20 C 0.5937(9) 0.6616(10) 0.8652(6) 0.034(3) Uani 1 1 d . . . . .
H20 H 0.642237 0.694137 0.847420 0.041 Uiso 1 1 calc R . . . .
C21 C 0.5499(9) 0.3284(15) 0.7683(6) 0.047(4) Uani 1 1 d . . . . .
C22 C 0.5261(9) 0.2218(10) 0.7663(6) 0.034(3) Uani 1 1 d . . . . .
H22A H 0.579282 0.188031 0.750362 0.041 Uiso 1 1 calc R . . . .
H22B H 0.516584 0.199191 0.805256 0.041 Uiso 1 1 calc R . . . .
C23 C 0.4578(9) 0.1841(11) 0.6707(4) 0.034(3) Uani 1 1 d . . . . .
C24 C 0.4053(8) 0.1180(9) 0.6437(4) 0.025(2) Uani 1 1 d . . . . .
H24 H 0.363283 0.081368 0.664380 0.030 Uiso 1 1 calc R . . . .
C25 C 0.4152(7) 0.1052(9) 0.5831(4) 0.024(2) Uani 1 1 d . . . . .
C26 C 0.3622(8) 0.0312(8) 0.5523(5) 0.026(2) Uani 1 1 d . . . . .
C27 C 0.4797(9) 0.1573(10) 0.5546(5) 0.032(3) Uani 1 1 d . . . . .
H27 H 0.485374 0.150646 0.514851 0.038 Uiso 1 1 calc R . . . .
C28 C 0.5382(8) 0.2215(12) 0.5844(5) 0.036(3) Uani 1 1 d . . . . .
C29 C 0.6097(8) 0.2814(9) 0.5536(5) 0.028(2) Uani 1 1 d . . . . .
C30 C 0.5262(8) 0.2348(9) 0.6444(5) 0.027(2) Uani 1 1 d . . . . .
H30 H 0.563930 0.276738 0.665169 0.033 Uiso 1 1 calc R . . . .
C31 C 0.1879(9) 0.1884(9) 0.7386(5) 0.029(3) Uani 1 1 d . . . . .
C32 C 0.0809(10) 0.1553(12) 0.7374(6) 0.045(4) Uani 1 1 d . . . . .
H32C H 0.041185 0.206704 0.749698 0.054 Uiso 1 1 calc R . . . .
H32D H 0.062616 0.139639 0.698058 0.054 Uiso 1 1 calc R . . . .
C33 C 0.0413(7) 0.0929(8) 0.8328(4) 0.020(2) Uani 1 1 d . . . . .
C34 C -0.0232(9) 0.0371(11) 0.8598(5) 0.034(3) Uani 1 1 d . . . . .
H34 H -0.052042 -0.012536 0.840435 0.041 Uiso 1 1 calc R . . . .
C35 C -0.0452(9) 0.0573(9) 0.9190(5) 0.027(2) Uani 1 1 d . . . . .
C36 C -0.1197(8) 0.0001(10) 0.9476(5) 0.031(3) Uani 1 1 d . . . . .
C37 C 0.0028(9) 0.1276(9) 0.9481(5) 0.030(3) Uani 1 1 d . . . . .
H37 H -0.008957 0.138211 0.986952 0.036 Uiso 1 1 calc R . . . .
C38 C 0.0692(10) 0.1829(9) 0.9194(6) 0.033(3) Uani 1 1 d . . . . .
C39 C 0.1250(8) 0.2586(10) 0.9518(5) 0.031(3) Uani 1 1 d . . . . .
C40 C 0.0876(8) 0.1662(8) 0.8624(6) 0.032(3) Uani 1 1 d . . . . .
H40 H 0.130903 0.203417 0.843111 0.038 Uiso 1 1 calc R . . . .
C42 C 0.750(2) 1.150(2) 0.8443(13) 0.072(5) Uani 0.7 1 d . U P A 1
H42A H 0.711554 1.204946 0.839231 0.109 Uiso 0.7 1 calc GR . P A 1
H42B H 0.805444 1.164869 0.866603 0.109 Uiso 0.7 1 calc GR . P A 1
H42C H 0.713737 1.103031 0.864079 0.109 Uiso 0.7 1 calc GR . P A 1
C47 C 0.3046(16) 0.4531(15) 0.6284(10) 0.076(6) Uani 1 1 d . U . . .
H47 H 0.259199 0.482843 0.650497 0.092 Uiso 1 1 calc R . . . .
C48 C 0.3912(19) 0.4288(19) 0.5320(12) 0.099(6) Uani 1 1 d . U . . .
H48A H 0.451258 0.415965 0.550411 0.149 Uiso 1 1 calc GR . . . .
H48B H 0.401099 0.461736 0.496536 0.149 Uiso 1 1 calc GR . . . .
H48C H 0.358867 0.371056 0.524079 0.149 Uiso 1 1 calc GR . . . .
C49 C 0.2757(17) 0.5611(18) 0.5457(12) 0.091(6) Uani 1 1 d . U . . .
H49A H 0.291709 0.619990 0.563130 0.136 Uiso 1 1 calc GR . . . .
H49B H 0.209624 0.548372 0.551129 0.136 Uiso 1 1 calc GR . . . .
H49C H 0.288515 0.563418 0.505165 0.136 Uiso 1 1 calc GR . . . .
O25 O 0.8057(15) 0.975(2) 0.7480(16) 0.055(4) Uani 0.7 1 d . U P A 1
O29 O 0.739(3) 0.496(2) 0.8611(15) 0.049(5) Uani 0.55 1 d . U P B 1
N5 N 0.7747(17) 1.1171(17) 0.7925(11) 0.070(4) Uani 0.7 1 d . U P A 1
N6 N 0.8321(17) 0.4642(17) 0.9396(10) 0.049(4) Uani 0.55 1 d . U P B 1
C41 C 0.7711(19) 1.0177(17) 0.7918(12) 0.060(4) Uani 0.7 1 d . U P A 1
H41 H 0.744458 0.984697 0.822085 0.072 Uiso 0.7 1 calc R . P A 1
C43 C 0.813(2) 1.181(2) 0.7401(13) 0.071(5) Uani 0.7 1 d . U P A 1
H43A H 0.852103 1.143822 0.715446 0.106 Uiso 0.7 1 calc GR . P A 1
H43B H 0.850101 1.231940 0.755638 0.106 Uiso 0.7 1 calc GR . P A 1
H43C H 0.760454 1.205509 0.718218 0.106 Uiso 0.7 1 calc GR . P A 1
C44 C 0.814(2) 0.448(2) 0.8802(12) 0.054(4) Uani 0.55 1 d . U P B 1
H44 H 0.849850 0.408041 0.857276 0.065 Uiso 0.55 1 calc R . P B 1
C45 C 0.776(2) 0.511(2) 0.9762(13) 0.052(4) Uani 0.55 1 d . U P B 1
H45A H 0.778660 0.481107 1.013325 0.078 Uiso 0.55 1 calc GR . P B 1
H45B H 0.712174 0.510439 0.961537 0.078 Uiso 0.55 1 calc GR . P B 1
H45C H 0.797968 0.574161 0.979770 0.078 Uiso 0.55 1 calc GR . P B 1
C46 C 0.912(2) 0.415(2) 0.9626(12) 0.052(4) Uani 0.55 1 d . U P B 1
H46A H 0.969192 0.445771 0.951173 0.077 Uiso 0.55 1 calc GR . P B 1
H46B H 0.911673 0.352098 0.948137 0.077 Uiso 0.55 1 calc GR . P B 1
H46C H 0.908980 0.413954 1.003955 0.077 Uiso 0.55 1 calc GR . P B 1
O26 O 0.780(4) 0.968(6) 0.749(4) 0.056(5) Uani 0.3 1 d D U P A 2
H26A H 0.802(11) 1.017(5) 0.724(8) 0.085 Uiso 0.3 1 d DR . P C 2
H26B H 0.711(5) 0.963(6) 0.756(11) 0.085 Uiso 0.3 1 d DR . P D 2
O30 O 0.726(3) 0.470(3) 0.8575(19) 0.052(5) Uani 0.45 1 d D U P B 2
H30A H 0.750(13) 0.526(6) 0.877(3) 0.079 Uiso 0.45 1 d DR . P E 2
H30B H 0.683(9) 0.429(10) 0.879(3) 0.079 Uiso 0.45 1 d DR . P F 2
O40 O 0.6189(14) 0.3414(15) 1.0887(8) 0.060(4) Uani 0.6 1 d . U P . .
N9 N 0.6195(16) 0.3073(18) 0.9868(10) 0.054(4) Uani 0.6 1 d . U P . .
C53 C 0.581(2) 0.347(2) 1.0380(12) 0.058(4) Uani 0.6 1 d . U P . .
H53 H 0.524643 0.379568 1.034296 0.070 Uiso 0.6 1 calc R . P . .
C54 C 0.701(2) 0.244(2) 1.0011(13) 0.060(4) Uani 0.6 1 d . U P . .
H54A H 0.702986 0.193921 0.973360 0.090 Uiso 0.6 1 calc GR . P . .
H54B H 0.693192 0.218191 1.038994 0.090 Uiso 0.6 1 calc GR . P . .
H54C H 0.759166 0.278554 0.999953 0.090 Uiso 0.6 1 calc GR . P . .
C55 C 0.5742(19) 0.319(2) 0.9343(10) 0.052(4) Uani 0.6 1 d . U P . .
H55A H 0.569541 0.259702 0.914971 0.078 Uiso 0.6 1 calc GR . P . .
H55B H 0.609709 0.361638 0.911128 0.078 Uiso 0.6 1 calc GR . P . .
H55C H 0.511819 0.343522 0.940171 0.078 Uiso 0.6 1 calc GR . 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
Cd1 O1 2.296(9) . ?
Cd1 O8 2.236(10) . ?
Cd1 O27 2.333(9) . ?
Cd1 O28 2.283(10) . ?
Cd1 N1 2.408(9) . ?
Cd1 O25 2.22(3) . ?
Cd1 O26 2.26(8) . ?
Cd2 O7 2.261(9) . ?
Cd2 O14 2.295(13) . ?
Cd2 O31 2.219(14) . ?
Cd2 O32 2.279(12) . ?
Cd2 N2 2.343(14) . ?
Cd2 O29 2.33(3) . ?
Cd2 O30 2.22(5) . ?
Cd3 O13 2.299(9) . ?
Cd3 O20 2.246(11) . ?
Cd3 O33 2.267(11) . ?
Cd3 O34 2.116(12) . ?
Cd3 O35 2.324(9) . ?
Cd3 N3 2.410(11) . ?
Cd4 O2 2.281(11) 1_445 ?
Cd4 O19 2.285(11) . ?
Cd4 O36 2.344(11) . ?
Cd4 O37 2.262(11) . ?
Cd4 O38 2.306(9) . ?
Cd4 N4 2.386(13) . ?
Cd5 O3 2.260(7) . ?
Cd5 O4 2.619(10) . ?
Cd5 O5 2.529(10) 2_746 ?
Cd5 O6 2.325(7) 2_746 ?
Cd5 O15 2.374(8) 2_656 ?
Cd5 O16 2.469(10) 2_656 ?
Cd5 O17 2.452(8) . ?
Cd5 O18 2.402(7) . ?
Cd6 O9 2.355(8) . ?
Cd6 O10 2.462(10) . ?
Cd6 O11 2.557(12) 2_647 ?
Cd6 O12 2.314(8) 2_647 ?
Cd6 O21 2.355(7) 2_557 ?
Cd6 O22 2.325(12) 2_557 ?
Cd6 O23 2.525(10) . ?
Cd6 O24 2.346(8) . ?
Cd6 C16 2.755(12) . ?
Cd6 C36 2.723(12) 2_557 ?
O1 C1 1.31(2) . ?
O2 C1 1.225(18) . ?
O3 C6 1.259(15) . ?
O4 C6 1.252(15) . ?
O5 C9 1.226(14) . ?
O6 C9 1.277(13) . ?
O7 C11 1.255(17) . ?
O8 C11 1.270(18) . ?
O9 C16 1.269(15) . ?
O10 C16 1.275(15) . ?
O11 C19 1.307(16) . ?
O12 C19 1.214(16) . ?
O13 C21 1.24(2) . ?
O14 C21 1.234(16) . ?
O15 C26 1.271(15) . ?
O16 C26 1.262(15) . ?
O17 C29 1.264(15) . ?
O18 C29 1.261(15) . ?
O19 C31 1.201(16) . ?
O20 C31 1.176(17) . ?
O21 C36 1.227(15) . ?
O22 C36 1.238(16) . ?
O23 C39 1.213(16) . ?
O24 C39 1.236(16) . ?
O33 C47 1.24(3) . ?
N1 C2 1.443(17) . ?
N1 C3 1.464(13) . ?
N2 C12 1.476(17) . ?
N2 C13 1.402(15) . ?
N3 C22 1.435(17) . ?
N3 C23 1.463(13) . ?
N4 C32 1.44(2) . ?
N4 C33 1.429(14) . ?
N7 C47 1.46(3) . ?
N7 C48 1.53(3) . ?
N7 C49 1.43(3) . ?
C1 C2 1.52(2) . ?
C3 C4 1.420(16) . ?
C3 C10 1.394(15) . ?
C4 C5 1.391(14) . ?
C5 C6 1.506(15) . ?
C5 C7 1.421(15) . ?
C7 C8 1.315(16) . ?
C8 C9 1.529(15) . ?
C8 C10 1.378(14) . ?
C11 C12 1.533(18) . ?
C13 C14 1.411(16) . ?
C13 C20 1.341(19) . ?
C14 C15 1.402(16) . ?
C15 C16 1.493(15) . ?
C15 C17 1.442(16) . ?
C17 C18 1.349(17) . ?
C18 C19 1.477(18) . ?
C18 C20 1.399(17) . ?
C21 C22 1.56(2) . ?
C23 C24 1.348(17) . ?
C23 C30 1.359(17) . ?
C24 C25 1.426(13) . ?
C25 C26 1.474(16) . ?
C25 C27 1.357(17) . ?
C27 C28 1.407(18) . ?
C28 C29 1.512(17) . ?
C28 C30 1.416(16) . ?
C31 C32 1.582(19) . ?
C33 C34 1.369(18) . ?
C33 C40 1.407(17) . ?
C34 C35 1.440(15) . ?
C35 C36 1.496(15) . ?
C35 C37 1.381(16) . ?
C37 C38 1.403(15) . ?
C38 C39 1.529(17) . ?
C38 C40 1.371(19) . ?
C42 N5 1.34(4) . ?
O25 C41 1.29(4) . ?
O29 C44 1.34(5) . ?
N5 C41 1.42(3) . ?
N5 C43 1.62(4) . ?
N6 C44 1.42(3) . ?
N6 C45 1.34(4) . ?
N6 C46 1.42(3) . ?
O40 C53 1.28(3) . ?
N9 C53 1.43(4) . ?
N9 C54 1.50(4) . ?
N9 C55 1.37(3) . ?

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
O1 Cd1 O27 89.1(4) . . ?
O1 Cd1 N1 73.1(3) . . ?
O8 Cd1 O1 178.6(4) . . ?
O8 Cd1 O27 92.3(4) . . ?
O8 Cd1 O28 90.0(4) . . ?
O8 Cd1 N1 107.1(4) . . ?
O8 Cd1 O26 85.8(18) . . ?
O27 Cd1 N1 89.8(3) . . ?
O28 Cd1 O1 88.6(3) . . ?
O28 Cd1 O27 172.5(4) . . ?
O28 Cd1 N1 96.3(4) . . ?
O25 Cd1 O1 84.6(7) . . ?
O25 Cd1 O8 95.2(7) . . ?
O25 Cd1 O27 88.0(10) . . ?
O25 Cd1 O28 84.6(10) . . ?
O25 Cd1 N1 157.6(7) . . ?
O26 Cd1 O1 94.1(18) . . ?
O26 Cd1 O27 86(2) . . ?
O26 Cd1 O28 87(2) . . ?
O26 Cd1 N1 166.7(19) . . ?
O7 Cd2 O14 177.8(4) . . ?
O7 Cd2 O32 87.5(4) . . ?
O7 Cd2 N2 74.8(4) . . ?
O7 Cd2 O29 91.5(7) . . ?
O14 Cd2 N2 105.1(4) . . ?
O14 Cd2 O29 90.8(7) . . ?
O31 Cd2 O7 91.6(7) . . ?
O31 Cd2 O14 88.5(7) . . ?
O31 Cd2 O32 91.0(5) . . ?
O31 Cd2 N2 166.4(7) . . ?
O31 Cd2 O29 85.3(11) . . ?
O32 Cd2 O14 90.2(4) . . ?
O32 Cd2 N2 89.5(4) . . ?
O32 Cd2 O29 176.1(10) . . ?
O29 Cd2 N2 93.8(11) . . ?
O30 Cd2 O7 101.7(9) . . ?
O30 Cd2 O14 80.5(9) . . ?
O30 Cd2 O31 85.1(14) . . ?
O30 Cd2 O32 170.0(11) . . ?
O30 Cd2 N2 96.5(13) . . ?
O13 Cd3 O35 86.3(4) . . ?
O13 Cd3 N3 73.0(4) . . ?
O20 Cd3 O13 172.7(4) . . ?
O20 Cd3 O33 91.2(5) . . ?
O20 Cd3 O35 92.1(4) . . ?
O20 Cd3 N3 99.8(4) . . ?
O33 Cd3 O13 90.8(5) . . ?
O33 Cd3 O35 174.7(6) . . ?
O33 Cd3 N3 97.0(4) . . ?
O34 Cd3 O13 98.6(5) . . ?
O34 Cd3 O20 88.5(5) . . ?
O34 Cd3 O33 87.2(5) . . ?
O34 Cd3 O35 88.8(4) . . ?
O34 Cd3 N3 170.6(4) . . ?
O35 Cd3 N3 86.5(4) . . ?
O2 Cd4 O19 173.6(3) 1_445 . ?
O2 Cd4 O36 94.0(4) 1_445 . ?
O2 Cd4 O38 90.4(4) 1_445 . ?
O2 Cd4 N4 101.6(4) 1_445 . ?
O19 Cd4 O36 86.0(4) . . ?
O19 Cd4 O38 90.3(4) . . ?
O19 Cd4 N4 72.0(3) . . ?
O36 Cd4 N4 86.0(4) . . ?
O37 Cd4 O2 87.9(5) . 1_445 ?
O37 Cd4 O19 98.5(5) . . ?
O37 Cd4 O36 85.4(5) . . ?
O37 Cd4 O38 88.5(5) . . ?
O37 Cd4 N4 167.6(5) . . ?
O38 Cd4 O36 172.4(4) . . ?
O38 Cd4 N4 99.3(4) . . ?
O3 Cd5 O4 52.9(3) . . ?
O3 Cd5 O5 88.9(3) . 2_746 ?
O3 Cd5 O6 126.5(3) . 2_746 ?
O3 Cd5 O15 120.4(4) . 2_656 ?
O3 Cd5 O16 85.4(3) . 2_656 ?
O3 Cd5 O17 131.6(3) . . ?
O3 Cd5 O18 77.7(3) . . ?
O5 Cd5 O4 85.9(4) 2_746 . ?
O6 Cd5 O4 84.6(3) 2_746 . ?
O6 Cd5 O5 53.2(3) 2_746 2_746 ?
O6 Cd5 O15 76.9(3) 2_746 2_656 ?
O6 Cd5 O16 131.0(3) 2_746 2_656 ?
O6 Cd5 O17 90.3(3) 2_746 . ?
O6 Cd5 O18 129.7(4) 2_746 . ?
O15 Cd5 O4 82.8(4) 2_656 . ?
O15 Cd5 O5 129.7(3) 2_656 2_746 ?
O15 Cd5 O16 54.2(3) 2_656 2_656 ?
O15 Cd5 O17 95.4(3) 2_656 . ?
O15 Cd5 O18 133.1(3) 2_656 . ?
O16 Cd5 O4 90.7(4) 2_656 . ?
O16 Cd5 O5 174.3(3) 2_656 2_746 ?
O17 Cd5 O4 174.9(3) . . ?
O17 Cd5 O5 91.7(4) . 2_746 ?
O17 Cd5 O16 92.0(3) . 2_656 ?
O18 Cd5 O4 130.4(3) . . ?
O18 Cd5 O5 89.8(3) . 2_746 ?
O18 Cd5 O16 88.9(4) . 2_656 ?
O18 Cd5 O17 54.0(3) . . ?
O9 Cd6 O10 54.9(3) . . ?
O9 Cd6 O11 84.9(4) . 2_647 ?
O9 Cd6 O23 130.0(3) . . ?
O9 Cd6 C16 27.3(3) . . ?
O9 Cd6 C36 119.0(4) . 2_557 ?
O10 Cd6 O11 96.2(4) . 2_647 ?
O10 Cd6 O23 174.7(4) . . ?
O10 Cd6 C16 27.6(3) . . ?
O10 Cd6 C36 93.0(4) . 2_557 ?
O11 Cd6 C16 90.3(4) 2_647 . ?
O11 Cd6 C36 155.2(4) 2_647 2_557 ?
O12 Cd6 O9 121.2(3) 2_647 . ?
O12 Cd6 O10 87.3(4) 2_647 . ?
O12 Cd6 O11 53.2(3) 2_647 2_647 ?
O12 Cd6 O21 78.0(3) 2_647 2_557 ?
O12 Cd6 O22 130.6(3) 2_647 2_557 ?
O12 Cd6 O23 87.9(4) 2_647 . ?
O12 Cd6 O24 126.0(4) 2_647 . ?
O12 Cd6 C16 105.3(4) 2_647 . ?
O12 Cd6 C36 104.5(3) 2_647 2_557 ?
O21 Cd6 O9 139.8(4) 2_557 . ?
O21 Cd6 O10 95.5(4) 2_557 . ?
O21 Cd6 O11 129.0(3) 2_557 2_647 ?
O21 Cd6 O23 81.2(4) 2_557 . ?
O21 Cd6 C16 119.2(4) 2_557 . ?
O21 Cd6 C36 26.7(3) 2_557 2_557 ?
O22 Cd6 O9 94.7(4) 2_557 . ?
O22 Cd6 O10 87.7(6) 2_557 . ?
O22 Cd6 O11 174.8(5) 2_557 2_647 ?
O22 Cd6 O21 53.6(3) 2_557 2_557 ?
O22 Cd6 O23 93.6(5) 2_557 . ?
O22 Cd6 O24 91.3(4) 2_557 . ?
O22 Cd6 C16 91.7(4) 2_557 . ?
O22 Cd6 C36 26.9(4) 2_557 2_557 ?
O23 Cd6 O11 82.8(6) . 2_647 ?
O23 Cd6 C16 157.3(3) . . ?
O23 Cd6 C36 85.9(4) . 2_557 ?
O24 Cd6 O9 78.4(3) . . ?
O24 Cd6 O10 132.9(3) . . ?
O24 Cd6 O11 83.5(4) . 2_647 ?
O24 Cd6 O21 121.0(3) . 2_557 ?
O24 Cd6 O23 52.2(3) . . ?
O24 Cd6 C16 105.6(3) . . ?
O24 Cd6 C36 106.6(4) . 2_557 ?
C36 Cd6 C16 107.9(4) 2_557 . ?
C1 O1 Cd1 113.4(9) . . ?
C1 O2 Cd4 119.9(12) . 1_665 ?
C6 O3 Cd5 100.6(6) . . ?
C6 O4 Cd5 84.0(7) . . ?
C9 O5 Cd5 88.1(7) . 2_756 ?
C9 O6 Cd5 96.4(6) . 2_756 ?
C11 O7 Cd2 116.5(8) . . ?
C11 O8 Cd1 114.3(9) . . ?
C16 O9 Cd6 94.2(7) . . ?
C16 O10 Cd6 89.1(8) . . ?
C19 O11 Cd6 86.0(8) . 2_657 ?
C19 O12 Cd6 99.7(8) . 2_657 ?
C21 O13 Cd3 115.3(11) . . ?
C21 O14 Cd2 114.0(13) . . ?
C26 O15 Cd5 94.3(7) . 2_646 ?
C26 O16 Cd5 90.1(7) . 2_646 ?
C29 O17 Cd5 91.0(7) . . ?
C29 O18 Cd5 93.4(7) . . ?
C31 O19 Cd4 118.5(8) . . ?
C31 O20 Cd3 119.6(10) . . ?
C36 O21 Cd6 93.6(7) . 2_547 ?
C36 O22 Cd6 94.8(9) . 2_547 ?
C39 O23 Cd6 88.1(8) . . ?
C39 O24 Cd6 96.1(8) . . ?
C47 O33 Cd3 121.2(15) . . ?
C2 N1 Cd1 105.7(8) . . ?
C2 N1 C3 114.3(10) . . ?
C3 N1 Cd1 113.4(7) . . ?
C12 N2 Cd2 105.4(8) . . ?
C13 N2 Cd2 111.4(10) . . ?
C13 N2 C12 116.7(11) . . ?
C22 N3 Cd3 108.0(8) . . ?
C22 N3 C23 116.2(10) . . ?
C23 N3 Cd3 108.4(8) . . ?
C32 N4 Cd4 105.2(8) . . ?
C33 N4 Cd4 111.2(8) . . ?
C33 N4 C32 118.0(11) . . ?
C47 N7 C48 119.9(19) . . ?
C49 N7 C47 119(2) . . ?
C49 N7 C48 117(2) . . ?
O1 C1 C2 120.0(13) . . ?
O2 C1 O1 123.5(16) . . ?
O2 C1 C2 115.9(17) . . ?
N1 C2 C1 115.2(12) . . ?
C4 C3 N1 118.7(9) . . ?
C10 C3 N1 120.9(10) . . ?
C10 C3 C4 120.1(10) . . ?
C5 C4 C3 118.2(10) . . ?
C4 C5 C6 118.4(10) . . ?
C4 C5 C7 120.0(10) . . ?
C7 C5 C6 121.4(10) . . ?
O3 C6 C5 119.2(10) . . ?
O4 C6 O3 122.1(10) . . ?
O4 C6 C5 118.7(11) . . ?
C8 C7 C5 119.4(10) . . ?
C7 C8 C9 120.7(9) . . ?
C7 C8 C10 123.7(11) . . ?
C10 C8 C9 115.3(10) . . ?
O5 C9 O6 121.5(10) . . ?
O5 C9 C8 119.2(10) . . ?
O6 C9 C8 119.1(9) . . ?
C8 C10 C3 118.5(10) . . ?
O7 C11 O8 127.3(13) . . ?
O7 C11 C12 118.8(13) . . ?
O8 C11 C12 113.8(13) . . ?
N2 C12 C11 114.5(13) . . ?
N2 C13 C14 119.0(11) . . ?
C20 C13 N2 122.4(11) . . ?
C20 C13 C14 118.5(11) . . ?
C15 C14 C13 120.3(11) . . ?
C14 C15 C16 120.0(10) . . ?
C14 C15 C17 118.2(10) . . ?
C17 C15 C16 121.7(10) . . ?
O9 C16 Cd6 58.5(6) . . ?
O9 C16 O10 121.8(11) . . ?
O9 C16 C15 119.4(10) . . ?
O10 C16 Cd6 63.3(7) . . ?
O10 C16 C15 118.7(11) . . ?
C15 C16 Cd6 175.7(9) . . ?
C18 C17 C15 120.3(11) . . ?
C17 C18 C19 122.3(11) . . ?
C17 C18 C20 119.2(12) . . ?
C20 C18 C19 118.5(11) . . ?
O11 C19 C18 117.6(11) . . ?
O12 C19 O11 120.8(13) . . ?
O12 C19 C18 121.6(11) . . ?
C13 C20 C18 123.3(11) . . ?
O13 C21 C22 122.6(13) . . ?
O14 C21 O13 128.8(19) . . ?
O14 C21 C22 108.2(16) . . ?
N3 C22 C21 111.7(12) . . ?
C24 C23 N3 119.6(10) . . ?
C24 C23 C30 123.7(10) . . ?
C30 C23 N3 116.7(11) . . ?
C23 C24 C25 119.0(10) . . ?
C24 C25 C26 120.9(10) . . ?
C27 C25 C24 119.0(11) . . ?
C27 C25 C26 119.9(10) . . ?
O15 C26 C25 118.1(10) . . ?
O16 C26 O15 121.3(11) . . ?
O16 C26 C25 120.5(11) . . ?
C25 C27 C28 120.8(11) . . ?
C27 C28 C29 121.9(10) . . ?
C27 C28 C30 119.4(12) . . ?
C30 C28 C29 118.5(11) . . ?
O17 C29 C28 119.5(10) . . ?
O18 C29 O17 121.5(10) . . ?
O18 C29 C28 118.9(10) . . ?
C23 C30 C28 117.7(11) . . ?
O19 C31 C32 117.3(12) . . ?
O20 C31 O19 128.8(14) . . ?
O20 C31 C32 113.9(13) . . ?
N4 C32 C31 113.5(12) . . ?
C34 C33 N4 119.8(10) . . ?
C34 C33 C40 121.3(10) . . ?
C40 C33 N4 118.9(10) . . ?
C33 C34 C35 118.2(12) . . ?
C34 C35 C36 118.4(11) . . ?
C37 C35 C34 119.9(11) . . ?
C37 C35 C36 121.6(10) . . ?
O21 C36 Cd6 59.7(6) . 2_547 ?
O21 C36 O22 117.8(11) . . ?
O21 C36 C35 120.4(11) . . ?
O22 C36 Cd6 58.3(7) . 2_547 ?
O22 C36 C35 121.8(11) . . ?
C35 C36 Cd6 177.0(10) . 2_547 ?
C35 C37 C38 120.3(10) . . ?
C37 C38 C39 120.6(11) . . ?
C40 C38 C37 119.8(11) . . ?
C40 C38 C39 119.5(11) . . ?
O23 C39 O24 122.7(12) . . ?
O23 C39 C38 120.7(11) . . ?
O24 C39 C38 116.5(11) . . ?
C38 C40 C33 120.3(10) . . ?
O33 C47 N7 117(2) . . ?
C41 O25 Cd1 134(2) . . ?
C44 O29 Cd2 119(3) . . ?
C42 N5 C41 110(3) . . ?
C42 N5 C43 125(2) . . ?
C41 N5 C43 125(2) . . ?
C44 N6 C46 114(3) . . ?
C45 N6 C44 127(2) . . ?
C45 N6 C46 119(2) . . ?
O25 C41 N5 118(3) . . ?
O29 C44 N6 111(3) . . ?
C53 N9 C54 111(2) . . ?
C55 N9 C53 121(3) . . ?
C55 N9 C54 128(3) . . ?
O40 C53 N9 126(3) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O32 H32A O18 0.979(7) 2.02(5) 2.862(15) 143(6) . yes
O35 H35B O9 0.979(7) 1.84(3) 2.784(16) 162(8) . yes
O36 H36A O15 0.981(7) 2.44(12) 2.817(14) 102(8) . yes


_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.581(13)
2 0.419(13)
####################################################################### 
# 
# 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_e18adb5
_database_code_depnum_ccdc_archive 'CCDC 2097429'
loop_
_audit_author_name
_audit_author_address
'Mary Mahon'
;University of Bath
United Kingdom
;
_audit_update_record             
;
2021-07-19 deposited with the CCDC.	2021-12-20 downloaded from the CCDC.
;
_audit_creation_date             2018-08-02
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C10 H11 Cd N O8'
_chemical_formula_sum            'C10 H11 Cd N O8'
_chemical_formula_weight         385.60
_chemical_melting_point          ?
_chemical_oxdiff_usercomment     'Light Brown Block'
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'
Cd Cd -0.8075 1.2024 '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'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.2467(6)
_cell_length_b                   8.5509(7)
_cell_length_c                   10.9978(6)
_cell_angle_alpha                101.892(6)
_cell_angle_beta                 95.728(5)
_cell_angle_gamma                114.776(8)
_cell_volume                     592.04(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3496
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      30.0720
_cell_measurement_theta_min      4.0560
_shelx_estimated_absorpt_T_max   0.859
_shelx_estimated_absorpt_T_min   0.563
_exptl_absorpt_coefficient_mu    1.886
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94691
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light brown'
_exptl_crystal_density_diffrn    2.163
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             380
_exptl_crystal_size_max          0.344
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.083
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_unetI/netI     0.0588
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.839
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5470
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.839
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.339
_diffrn_reflns_theta_min         3.348
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0734
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.839
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2721
_reflns_number_total             2988
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.953
_refine_diff_density_min         -0.711
_refine_diff_density_rms         0.147
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         2988
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0335
_refine_ls_restrained_S_all      1.068
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0162P)²+0.3140P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0636
_refine_ls_wR_factor_ref         0.0668
_refine_special_details          
;
The asymmetric unit contains one full-occupancy cadmium 
centre, one 3-carboxy-5-((carboxylatomethyl)amino)benzoate ligand 
(H-5-CMAI) and two co-ordinated waters. Oxygen and nitrogen bound 
hydrogens were readily located and each refined at a distance of 
0.98Å from the relevant parent atom. All O- and N- bound 
hydrogen atoms are implicated in hydrogen bonding 
the result of which is formation of 1-D polymers in the gross structure.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 N1-H1
 0.98 with sigma of 0.005
 O8-H8B = O8-H8A
 0.98 with sigma of 0.005
 O5-H5
 0.98 with sigma of 0.005
 O7-H7B = O7-H7A
 0.98 with sigma of 0.005
3.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C7(H7), C10(H10)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
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 0.86632(3) 0.33441(3) 0.08663(2) 0.00983(8) Uani 1 1 d . . . . .
O1 O 0.8896(3) 0.5876(3) 0.0321(2) 0.0155(5) Uani 1 1 d . . . . .
O2 O 0.7807(4) 0.7915(3) 0.0253(2) 0.0166(5) Uani 1 1 d . . . . .
O3 O 1.0165(3) 0.7558(3) 0.6317(2) 0.0129(5) Uani 1 1 d . . . . .
O4 O 0.8913(3) 0.5466(3) 0.7354(2) 0.0150(5) Uani 1 1 d . . . . .
O5 O 0.2381(4) 0.0199(3) 0.5434(2) 0.0182(5) Uani 1 1 d D . . . .
H5 H 0.134(7) -0.101(3) 0.538(5) 0.09(2) Uiso 1 1 d D . . . .
O6 O 0.1559(3) -0.1046(3) 0.3327(2) 0.0174(5) Uani 1 1 d . . . . .
O7 O 0.7352(3) 0.0732(3) 0.1455(2) 0.0131(5) Uani 1 1 d D . . . .
H7A H 0.762(6) -0.026(3) 0.104(3) 0.032(12) Uiso 1 1 d D . . . .
H7B H 0.820(5) 0.127(5) 0.2317(15) 0.046(13) Uiso 1 1 d D . . . .
O8 O 0.6700(4) 0.1747(3) -0.1149(2) 0.0220(6) Uani 1 1 d D . . . .
H8A H 0.747(6) 0.166(6) -0.182(3) 0.062(16) Uiso 1 1 d D . . . .
H8B H 0.530(3) 0.075(5) -0.141(5) 0.075(18) Uiso 1 1 d D . . . .
N1 N 0.6155(4) 0.4239(3) 0.1716(2) 0.0092(5) Uani 1 1 d D . . . .
H1 H 0.490(3) 0.332(3) 0.111(2) 0.010(9) Uiso 1 1 d D . . . .
C1 C 0.7834(5) 0.6667(4) 0.0661(3) 0.0123(6) Uani 1 1 d . . . . .
C2 C 0.6549(5) 0.6067(4) 0.1646(3) 0.0127(7) Uani 1 1 d . . . . .
H2A H 0.7275 0.6909 0.2474 0.015 Uiso 1 1 calc R . . . .
H2B H 0.5228 0.6087 0.1434 0.015 Uiso 1 1 calc R . . . .
C3 C 0.5999(5) 0.3925(4) 0.2944(3) 0.0099(6) Uani 1 1 d . . . . .
C4 C 0.7473(5) 0.5117(4) 0.4030(3) 0.0100(6) Uani 1 1 d . . . . .
H4 H 0.8539 0.6177 0.3977 0.012 Uiso 1 1 calc R . . . .
C5 C 0.7353(4) 0.4723(4) 0.5195(3) 0.0085(6) Uani 1 1 d . . . . .
C6 C 0.8934(5) 0.6016(4) 0.6370(3) 0.0095(6) Uani 1 1 d . . . . .
C7 C 0.5792(5) 0.3123(4) 0.5276(3) 0.0099(6) Uani 1 1 d . . . . .
H7 H 0.5736 0.2852 0.6052 0.012 Uiso 1 1 calc R . . . .
C8 C 0.4321(5) 0.1934(4) 0.4200(3) 0.0087(6) Uani 1 1 d . . . . .
C9 C 0.2613(5) 0.0214(4) 0.4249(3) 0.0126(7) Uani 1 1 d . . . . .
C10 C 0.4407(5) 0.2335(4) 0.3027(3) 0.0094(6) Uani 1 1 d . . . . .
H10 H 0.3407 0.1543 0.2306 0.011 Uiso 1 1 calc R . . . .


_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 O1 2.307(2) . ?
Cd1 O1 2.260(2) 2_765 ?
Cd1 O4 2.224(2) 2_766 ?
Cd1 O7 2.291(2) . ?
Cd1 O8 2.301(2) . ?
Cd1 N1 2.444(3) . ?
O1 Cd1 2.260(2) 2_765 ?
O1 C1 1.257(4) . ?
O2 C1 1.246(4) . ?
O3 C6 1.263(4) . ?
O4 Cd1 2.224(2) 2_766 ?
O4 C6 1.265(4) . ?
O5 C9 1.333(4) . ?
O6 C9 1.216(4) . ?
N1 C2 1.487(4) . ?
N1 C3 1.437(4) . ?
C1 C2 1.528(4) . ?
C3 C4 1.392(4) . ?
C3 C10 1.394(4) . ?
C4 C5 1.392(4) . ?
C5 C6 1.503(4) . ?
C5 C7 1.390(4) . ?
C7 C8 1.383(4) . ?
C8 C9 1.490(4) . ?
C8 C10 1.402(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cd1 O1 71.36(9) 2_765 . ?
O1 Cd1 O7 125.71(8) 2_765 . ?
O1 Cd1 O8 78.71(8) 2_765 . ?
O1 Cd1 N1 69.92(8) . . ?
O1 Cd1 N1 141.25(8) 2_765 . ?
O4 Cd1 O1 91.45(8) 2_766 2_765 ?
O4 Cd1 O1 101.42(8) 2_766 . ?
O4 Cd1 O7 87.60(8) 2_766 . ?
O4 Cd1 O8 164.52(9) 2_766 . ?
O4 Cd1 N1 97.25(9) 2_766 . ?
O7 Cd1 O1 160.92(8) . . ?
O7 Cd1 O8 88.53(9) . . ?
O7 Cd1 N1 92.45(8) . . ?
O8 Cd1 O1 86.84(9) . . ?
O8 Cd1 N1 97.89(9) . . ?
Cd1 O1 Cd1 108.64(9) 2_765 . ?
C1 O1 Cd1 127.3(2) . 2_765 ?
C1 O1 Cd1 124.1(2) . . ?
C6 O4 Cd1 128.25(19) . 2_766 ?
C2 N1 Cd1 112.24(17) . . ?
C3 N1 Cd1 109.8(2) . . ?
C3 N1 C2 115.8(2) . . ?
O1 C1 C2 117.3(3) . . ?
O2 C1 O1 123.5(3) . . ?
O2 C1 C2 119.2(3) . . ?
N1 C2 C1 112.7(3) . . ?
C4 C3 N1 121.3(3) . . ?
C4 C3 C10 119.8(3) . . ?
C10 C3 N1 118.8(3) . . ?
C3 C4 C5 120.0(3) . . ?
C4 C5 C6 120.0(3) . . ?
C7 C5 C4 120.3(3) . . ?
C7 C5 C6 119.7(3) . . ?
O3 C6 O4 124.7(3) . . ?
O3 C6 C5 118.7(3) . . ?
O4 C6 C5 116.6(3) . . ?
C8 C7 C5 119.9(3) . . ?
C7 C8 C9 121.6(3) . . ?
C7 C8 C10 120.2(3) . . ?
C10 C8 C9 118.3(3) . . ?
O5 C9 C8 112.0(3) . . ?
O6 C9 O5 123.4(3) . . ?
O6 C9 C8 124.6(3) . . ?
C3 C10 C8 119.8(3) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O5 H5 O3 0.979(5) 1.76(4) 2.607(3) 143(5) 1_445
O7 H7A O2 0.978(5) 1.691(7) 2.665(3) 174(4) 1_545
O7 H7B O3 0.978(5) 1.640(9) 2.611(3) 171(4) 2_766
O7 H7B O4 0.978(5) 2.62(4) 3.126(3) 113(3) 2_766
O8 H8A O6 0.978(5) 1.923(12) 2.887(3) 168(4) 2_655
O8 H8B O7 0.978(5) 1.793(16) 2.742(3) 163(5) 2_655
N1 H1 O2 0.977(5) 2.056(12) 3.002(4) 162(3) 2_665


_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_s18adb28
_database_code_depnum_ccdc_archive 'CCDC 2097430'
loop_
_audit_author_name
_audit_author_address
'Mary Mahon'
;University of Bath
United Kingdom
;
_audit_update_record             
;
2021-07-19 deposited with the CCDC.	2021-12-20 downloaded from the CCDC.
;
_audit_creation_date             2018-08-17
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelxl_version_number           2014-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C20 H20 Cd3 N2 O16, 4(H2 O)'
_chemical_formula_sum            'C20 H28 Cd3 N2 O20'
_chemical_formula_weight         953.64
_chemical_melting_point          ?
_chemical_oxdiff_usercomment     'Colourless Block'
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'
Cd Cd 0.1185 4.6533 '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'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.7777(2)
_cell_length_b                   8.9715(4)
_cell_length_c                   11.4851(4)
_cell_angle_alpha                67.353(4)
_cell_angle_beta                 75.848(3)
_cell_angle_gamma                70.505(3)
_cell_volume                     690.98(5)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    8998
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.3890
_cell_measurement_theta_min      4.1840
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    19.211
_exptl_absorpt_correction_T_min  0.30382
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.292
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             466
_exptl_crystal_size_max          0.038
_exptl_crystal_size_mid          0.028
_exptl_crystal_size_min          0.025
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            13561
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.349
_diffrn_reflns_theta_min         4.209
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1150
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2639
_reflns_number_total             2755
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.506
_refine_diff_density_min         -0.619
_refine_diff_density_rms         0.102
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         2755
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0216
_refine_ls_R_factor_gt           0.0199
_refine_ls_restrained_S_all      1.024
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0263P)²+0.6327P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0489
_refine_ls_wR_factor_ref         0.0496
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 O8-H8B = O8-H8A = O7_$1-H7A_$1 = O7_$1-H7B_$1
 0.98 with sigma of 0.005
 N1-H1
 0.98 with sigma of 0.005
 O9-H9B = O9-H9A
 0.98 with sigma of 0.005
 O10-H10A = O10-H10B
 0.98 with sigma of 0.02
 H10B-H10A
 1.5 with sigma of 0.1
 O10-H10A
 0.98 with sigma of 0.02
 H10A-H10B
 1.52 with sigma of 0.01
3.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B)
3.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C7(H7), C4(H4)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
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
Cd2 Cd 0.5000 -0.5000 1.0000 0.01199(7) Uani 1 2 d S T P . .
Cd1 Cd 0.74107(2) -0.19538(2) 0.68505(2) 0.01153(6) Uani 1 1 d . . . . .
O3 O -0.2344(2) 0.5603(2) 0.87481(17) 0.0144(4) Uani 1 1 d . . . . .
O1 O -0.0540(3) -0.1350(2) 1.47237(18) 0.0201(4) Uani 1 1 d . . . . .
O2 O -0.3127(3) 0.0492(2) 1.50948(17) 0.0190(4) Uani 1 1 d . . . . .
O5 O 0.4819(3) -0.0326(2) 0.76985(17) 0.0168(4) Uani 1 1 d . . . . .
O7 O 0.5761(3) -0.2978(2) 0.60780(18) 0.0173(4) Uani 1 1 d D . . . .
O4 O -0.0243(3) 0.5427(2) 0.71105(17) 0.0202(4) Uani 1 1 d . . . . .
O8 O 0.4142(3) -0.4983(2) 0.82358(18) 0.0187(4) Uani 1 1 d D . . . .
O6 O 0.4076(3) -0.2261(2) 0.9519(2) 0.0241(4) Uani 1 1 d . . . . .
C1 C -0.1649(4) 0.0054(3) 1.4398(2) 0.0151(5) Uani 1 1 d . . . . .
C9 C 0.3930(3) -0.0781(3) 0.8793(2) 0.0130(5) Uani 1 1 d . . . . .
C10 C 0.2186(3) 0.0142(3) 1.0622(2) 0.0131(5) Uani 1 1 d . . . . .
H10 H 0.2822 -0.0883 1.1142 0.016 Uiso 1 1 calc R . . . .
C7 C 0.1570(3) 0.2055(3) 0.8514(2) 0.0131(5) Uani 1 1 d . . . . .
H7 H 0.1817 0.2330 0.7633 0.016 Uiso 1 1 calc R . . . .
C2 C -0.1281(3) 0.1353(3) 1.3114(2) 0.0138(5) Uani 1 1 d . . . . .
H2A H -0.2110 0.1477 1.2554 0.017 Uiso 1 1 calc R . . . .
H2B H -0.1521 0.2427 1.3223 0.017 Uiso 1 1 calc R . . . .
C8 C 0.2538(3) 0.0532(3) 0.9305(2) 0.0127(5) Uani 1 1 d . . . . .
C4 C -0.0106(3) 0.2782(3) 1.0388(2) 0.0119(5) Uani 1 1 d . . . . .
H4 H -0.0989 0.3535 1.0748 0.014 Uiso 1 1 calc R . . . .
C3 C 0.0893(3) 0.1273(3) 1.1164(2) 0.0118(5) Uani 1 1 d . . . . .
C5 C 0.0220(3) 0.3159(3) 0.9072(2) 0.0128(5) Uani 1 1 d . . . . .
C6 C -0.0850(3) 0.4801(3) 0.8257(2) 0.0130(5) Uani 1 1 d . . . . .
N1 N 0.0645(3) 0.0862(3) 1.2523(2) 0.0137(4) Uani 1 1 d D . . . .
O9 O 0.5493(3) 0.2815(3) 0.6848(2) 0.0282(5) Uani 1 1 d D . . . .
O10 O 0.2677(3) 0.5110(3) 0.5261(2) 0.0357(5) Uani 1 1 d D . . . .
H8A H 0.463(6) -0.418(4) 0.748(3) 0.056(13) Uiso 1 1 d D . . . .
H8B H 0.460(7) -0.608(3) 0.813(5) 0.070(16) Uiso 1 1 d D . . . .
H7A H 0.478(4) -0.211(4) 0.561(4) 0.047(12) Uiso 1 1 d D . . . .
H7B H 0.657(5) -0.378(4) 0.566(4) 0.052(13) Uiso 1 1 d D . . . .
H1 H 0.103(5) -0.0362(8) 1.288(3) 0.028(9) Uiso 1 1 d D . . . .
H9A H 0.524(6) 0.174(3) 0.704(4) 0.037(11) Uiso 1 1 d D . . . .
H9B H 0.443(6) 0.341(7) 0.638(5) 0.10(2) Uiso 1 1 d D . . . .
H10A H 0.177(3) 0.558(4) 0.469(2) 0.017(8) Uiso 1 1 d D . . . .
H10B H 0.190(5) 0.516(7) 0.608(2) 0.086(19) Uiso 1 1 d 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
Cd2 O3 2.3072(17) 2_557 ?
Cd2 O3 2.3072(17) 1_645 ?
Cd2 O8 2.2762(19) . ?
Cd2 O8 2.2762(19) 2_647 ?
Cd2 O6 2.1979(18) . ?
Cd2 O6 2.1979(18) 2_647 ?
Cd1 O3 2.4158(17) 1_645 ?
Cd1 O1 2.5404(19) 1_654 ?
Cd1 O2 2.3340(18) 1_654 ?
Cd1 O5 2.3054(18) . ?
Cd1 O7 2.2910(18) . ?
Cd1 O4 2.4091(18) 1_645 ?
Cd1 N1 2.415(2) 2_657 ?
O3 Cd2 2.3072(17) 1_465 ?
O3 Cd1 2.4158(17) 1_465 ?
O3 C6 1.273(3) . ?
O1 Cd1 2.5404(19) 1_456 ?
O1 C1 1.242(3) . ?
O2 Cd1 2.3341(18) 1_456 ?
O2 C1 1.267(3) . ?
O5 C9 1.262(3) . ?
O4 Cd1 2.4091(18) 1_465 ?
O4 C6 1.255(3) . ?
O6 C9 1.251(3) . ?
C1 C2 1.519(3) . ?
C9 C8 1.509(3) . ?
C10 C8 1.392(4) . ?
C10 C3 1.389(3) . ?
C7 C8 1.396(3) . ?
C7 C5 1.400(3) . ?
C2 N1 1.480(3) . ?
C4 C3 1.392(3) . ?
C4 C5 1.393(3) . ?
C3 N1 1.437(3) . ?
C5 C6 1.497(3) . ?
N1 Cd1 2.414(2) 2_657 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Cd2 O3 180.00(5) 1_645 2_557 ?
O8 Cd2 O3 87.67(7) . 1_645 ?
O8 Cd2 O3 92.33(7) . 2_557 ?
O8 Cd2 O3 87.67(7) 2_647 2_557 ?
O8 Cd2 O3 92.33(7) 2_647 1_645 ?
O8 Cd2 O8 180.0 . 2_647 ?
O6 Cd2 O3 82.04(7) . 1_645 ?
O6 Cd2 O3 82.05(7) 2_647 2_557 ?
O6 Cd2 O3 97.96(7) . 2_557 ?
O6 Cd2 O3 97.95(7) 2_647 1_645 ?
O6 Cd2 O8 85.55(7) 2_647 . ?
O6 Cd2 O8 94.45(7) . . ?
O6 Cd2 O8 94.45(7) 2_647 2_647 ?
O6 Cd2 O8 85.55(7) . 2_647 ?
O6 Cd2 O6 180.0 2_647 . ?
O3 Cd1 O1 131.74(6) 1_645 1_654 ?
O2 Cd1 O3 174.43(6) 1_654 1_645 ?
O2 Cd1 O1 53.60(6) 1_654 1_654 ?
O2 Cd1 O4 131.28(6) 1_654 1_645 ?
O2 Cd1 N1 89.33(7) 1_654 2_657 ?
O5 Cd1 O3 95.37(6) . 1_645 ?
O5 Cd1 O1 132.75(6) . 1_654 ?
O5 Cd1 O2 79.44(7) . 1_654 ?
O5 Cd1 O4 149.28(6) . 1_645 ?
O5 Cd1 N1 90.64(7) . 2_657 ?
O7 Cd1 O3 90.34(6) . 1_645 ?
O7 Cd1 O1 89.95(6) . 1_654 ?
O7 Cd1 O2 88.02(7) . 1_654 ?
O7 Cd1 O5 93.67(7) . . ?
O7 Cd1 O4 87.85(7) . 1_645 ?
O7 Cd1 N1 174.45(7) . 2_657 ?
O4 Cd1 O3 53.92(6) 1_645 1_645 ?
O4 Cd1 O1 77.87(6) 1_645 1_654 ?
O4 Cd1 N1 90.23(7) 1_645 2_657 ?
N1 Cd1 O3 92.75(7) 2_657 1_645 ?
N1 Cd1 O1 84.55(7) 2_657 1_654 ?
Cd2 O3 Cd1 118.97(7) 1_465 1_465 ?
C6 O3 Cd2 136.30(16) . 1_465 ?
C6 O3 Cd1 92.59(14) . 1_465 ?
C1 O1 Cd1 87.14(15) . 1_456 ?
C1 O2 Cd1 96.07(15) . 1_456 ?
C9 O5 Cd1 126.48(16) . . ?
C6 O4 Cd1 93.37(15) . 1_465 ?
C9 O6 Cd2 154.66(18) . . ?
O1 C1 O2 123.0(2) . . ?
O1 C1 C2 120.6(2) . . ?
O2 C1 C2 116.4(2) . . ?
O5 C9 C8 119.2(2) . . ?
O6 C9 O5 125.7(2) . . ?
O6 C9 C8 115.1(2) . . ?
C3 C10 C8 120.5(2) . . ?
C8 C7 C5 118.7(2) . . ?
N1 C2 C1 111.3(2) . . ?
C10 C8 C9 117.2(2) . . ?
C10 C8 C7 120.4(2) . . ?
C7 C8 C9 122.4(2) . . ?
C3 C4 C5 119.8(2) . . ?
C10 C3 C4 119.8(2) . . ?
C10 C3 N1 118.7(2) . . ?
C4 C3 N1 121.5(2) . . ?
C7 C5 C6 120.3(2) . . ?
C4 C5 C7 120.9(2) . . ?
C4 C5 C6 118.8(2) . . ?
O3 C6 C5 119.5(2) . . ?
O4 C6 O3 119.8(2) . . ?
O4 C6 C5 120.6(2) . . ?
C2 N1 Cd1 110.43(15) . 2_657 ?
C3 N1 Cd1 111.11(15) . 2_657 ?
C3 N1 C2 115.2(2) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O8 H8A O7 0.978(5) 1.770(9) 2.742(3) 172(4) .
O8 H8B O9 0.979(5) 1.94(3) 2.787(3) 143(4) 1_545
O7 H7A O2 0.978(5) 1.667(8) 2.641(3) 173(4) 2_557
O7 H7B O10 0.978(5) 1.760(17) 2.701(3) 160(4) 2_656
N1 H1 O1 0.978(5) 2.18(3) 2.719(3) 113(2) .
O9 H9A O5 0.976(5) 1.825(9) 2.791(3) 170(4) .
O9 H9B O10 0.978(5) 1.95(2) 2.900(4) 163(6) .
O10 H10B O4 0.990(19) 1.80(3) 2.726(3) 155(3) .


_olex2_submission_special_instructions 'No special instructions were received'
