# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_Compound1
_database_code_depnum_ccdc_archive 'CCDC 1583251'
_audit_update_record             
;
2018-06-10 deposited with the CCDC.
2018-07-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014

_chemical_name_systematic        
"poly-{[tris(mu7-1,3,5-tris(4-carboxyphenyl)benzene-kO:kO':kO'':kO''':k2O'''',O''''':kO'''':kO''''')bis(mu9-1,3,5-tris(4-carboxyphenyl)benzene-kO:kO:kO':kO'':kO'':kO''':kO'''':kO'''':kO''''')(mu6-1,3,5-tris(4-carboxyphenyl)benzene-kO:kO':kO'':kO''':kO'''':kO''''')nonakis(dimethylformamide)octadecacalcium(II)] heneicosa(dimetylfomramide)}"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C63 H51 Ca3 N3 O15, 7 (C3 H7 N O)'
_chemical_formula_sum            'C84 H100 Ca3 N10 O22'
_chemical_formula_weight         1721.97

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'
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_H-M_alt        'R 3 :H'
_space_group_name_Hall           'R 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   28.5523(8)
_cell_length_b                   28.5523(8)
_cell_length_c                   28.3085(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     19986.2(13)
_cell_formula_units_Z            9
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    47209
_cell_measurement_theta_min      2.295
_cell_measurement_theta_max      28.730

# SQUEEZE RESULTS (Version = 160617)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.008 -0.005 0.275 7916 605 ' '
# Missing Reflections Below sin(th)/lambda = 0.25
loop_
_platon_missing_refln_index_h
_platon_missing_refln_index_k
_platon_missing_refln_index_l
_platon_missing_refln_theta
-1 2 0 1.426
-1 1 1 1.093
0 2 1 1.797
0 1 2 1.658
-2 2 2 2.187
0 0 3 2.158
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
TITL shelx     R 3 :h       R = 0.06
CELL   28.5523   28.5523   28.3085     90.00     90.00    120.00
SPGR R3
# Solvent Accessible Volume =      7911
# Electrons Found in S.A.V. =       600
# Note: Atoms in Void are Labelled as Cxxx and Qxxx for all Others
Q101 0.859 0.901 0.562 !       1.28 eA-3
C102 0.564 0.798 0.617 !       0.76 eA-3
C103 0.648 0.414 0.561 !       0.75 eA-3
C104 0.993 0.012 0.335 !       0.71 eA-3
C105 0.718 0.273 0.220 !       0.71 eA-3
C106 0.390 0.724 0.547 !       0.70 eA-3
Q107 0.437 0.366 0.319 !       0.70 eA-3
C108 0.907 0.975 0.962 !       0.70 eA-3
Q109 0.728 0.311 0.904 !       0.69 eA-3
C110 0.430 0.750 0.634 !       0.69 eA-3
C111 0.789 0.008 0.064 !       0.69 eA-3
Q112 0.868 0.958 0.345 !       0.68 eA-3
C113 0.016 0.889 0.907 !       0.68 eA-3
C114 0.460 0.367 0.344 !       0.68 eA-3
C115 0.920 0.502 0.335 !       0.67 eA-3
Q116 0.672 0.383 0.671 !       0.67 eA-3
C117 0.029 0.633 0.133 !       0.66 eA-3
Q118 0.945 0.603 0.328 !       0.66 eA-3
C119 0.947 0.971 0.232 !       0.66 eA-3
C120 0.172 0.719 0.648 !       0.65 eA-3
Q121 0.947 0.164 0.914 !       0.65 eA-3
C122 0.999 0.999 0.930 !       0.65 eA-3
C123 0.978 0.975 0.256 !       0.63 eA-3
C124 0.642 0.211 0.270 !       0.62 eA-3
Q125 0.813 0.780 0.592 !       0.62 eA-3
C126 0.009 0.897 0.938 !       0.62 eA-3
Q127 0.023 0.866 0.899 !       0.61 eA-3
C128 0.978 0.986 0.898 !       0.61 eA-3
C129 0.290 0.523 0.633 !       0.60 eA-3
C130 0.922 0.008 0.861 !       0.60 eA-3
Q131 0.436 0.364 0.290 !       0.60 eA-3
Q132 0.844 0.976 0.898 !       0.60 eA-3
C133 0.042 0.976 0.264 !       0.60 eA-3
C134 0.687 0.210 0.290 !       0.60 eA-3
Q135 0.501 0.783 0.271 !       0.60 eA-3
C136 0.298 0.664 0.914 !       0.59 eA-3
Q137 0.486 0.945 0.173 !       0.59 eA-3
Q138 0.720 0.484 0.573 !       0.59 eA-3
Q139 0.734 0.900 0.522 !       0.59 eA-3
C140 0.492 0.470 0.375 !       0.59 eA-3
C141 0.891 0.116 0.961 !       0.59 eA-3
Q142 0.467 0.335 0.079 !       0.59 eA-3
Q143 0.922 0.803 0.647 !       0.58 eA-3
C144 0.664 0.329 0.641 !       0.58 eA-3
Q145 0.616 0.961 0.643 !       0.58 eA-3
C146 0.967 0.837 0.964 !       0.58 eA-3
Q147 0.157 0.601 0.986 !       0.58 eA-3
C148 0.720 0.034 0.023 !       0.58 eA-3
Q149 0.220 0.813 0.623 !       0.58 eA-3
Q150 0.468 0.344 0.974 !       0.57 eA-3
C151 0.625 0.331 0.540 !       0.57 eA-3
C152 0.974 0.733 0.026 !       0.57 eA-3
Q153 0.070 0.898 0.336 !       0.57 eA-3
C154 0.773 0.485 0.248 !       0.57 eA-3
Q155 0.030 0.212 0.572 !       0.57 eA-3
Q156 0.290 0.320 0.836 !       0.57 eA-3
C157 0.945 0.077 0.244 !       0.57 eA-3
C158 0.607 0.243 0.540 !       0.57 eA-3
C159 0.960 0.985 0.312 !       0.56 eA-3
Q160 0.936 0.695 0.657 !       0.56 eA-3
Q161 0.627 0.938 0.023 !       0.56 eA-3
C162 0.174 0.218 0.640 !       0.55 eA-3
C163 0.211 0.187 0.033 !       0.55 eA-3
Q164 0.944 0.655 0.111 !       0.55 eA-3
Q165 0.975 0.630 0.500 !       0.55 eA-3
Q166 0.579 0.966 0.392 !       0.55 eA-3
Q167 0.596 0.953 0.672 !       0.55 eA-3
Q168 0.118 0.713 0.140 !       0.55 eA-3
Q169 0.244 0.360 0.312 !       0.55 eA-3
C170 0.836 0.891 0.922 !       0.55 eA-3
C171 0.007 0.781 0.023 !       0.55 eA-3
Q172 0.662 0.383 0.134 !       0.55 eA-3
Q173 0.604 0.960 0.477 !       0.55 eA-3
Q174 0.534 0.158 0.344 !       0.55 eA-3
Q175 0.095 0.773 0.499 !       0.54 eA-3
C176 0.405 0.398 0.375 !       0.54 eA-3
C177 0.322 0.678 0.891 !       0.54 eA-3
C178 0.390 0.366 0.819 !       0.54 eA-3
Q179 0.968 0.853 0.281 !       0.54 eA-3
Q180 0.616 0.054 0.330 !       0.54 eA-3
C181 0.258 0.610 0.982 !       0.54 eA-3
C182 0.735 0.213 0.843 !       0.54 eA-3
Q183 0.944 0.608 0.742 !       0.54 eA-3
C184 0.124 0.149 0.361 !       0.54 eA-3
C185 0.023 0.904 0.969 !       0.53 eA-3
Q186 0.289 0.732 0.689 !       0.53 eA-3
C187 0.758 0.445 0.642 !       0.53 eA-3
Q188 0.842 0.570 0.938 !       0.53 eA-3
Q189 0.678 0.031 0.336 !       0.53 eA-3
C190 0.594 0.330 0.610 !       0.53 eA-3
Q191 0.415 0.617 0.001 !       0.53 eA-3
C192 0.374 0.595 0.579 !       0.52 eA-3
C193 0.953 0.474 0.392 !       0.52 eA-3
C194 0.913 0.563 0.375 !       0.52 eA-3
Q195 0.314 0.345 0.342 !       0.52 eA-3
Q196 0.211 0.267 0.718 !       0.52 eA-3
Q197 0.860 0.946 0.892 !       0.52 eA-3
C198 0.053 0.672 0.148 !       0.52 eA-3
Q199 0.398 0.265 0.015 !       0.52 eA-3
;


_exptl_crystal_description       prismatic
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_density_method    none
_exptl_crystal_F_000             8190
_exptl_absorpt_coefficient_mu    0.262
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
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)
;
_exptl_absorpt_correction_T_min  0.920
_exptl_absorpt_correction_T_max  0.960

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Venture'
_diffrn_measurement_method       ω
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            47209
_diffrn_reflns_av_unetI/netI     0.0924
_diffrn_reflns_av_R_equivalents  0.0589
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         2.295
_diffrn_reflns_theta_max         28.730
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             20969
_reflns_number_gt                14558
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_max     0.994
_reflns_Friedel_fraction_full    0.999

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;Refined as a 2-component inversion twin. Moreover, crystal structure of this 
compound contains many disordered DMF molecules occupying the voids. 
In spite of all efforts to refine them, almost no residual peaks were found 
in the Fourier difference, so SQUEEZE routine was applied and the corresponding 
hkl file was employed during the last cycles of the refinement. This is the reason
why chemical formula does not fit the crystallographic formula.
On the other hand, some restraints have been used to refine anisotropic displacment
paramters of atoms belonging to coordinated DMF molecules, because they are affected
by the disorder present in the voids of the structure.,SQUEEZE
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0993P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.05(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         20969
_refine_ls_number_parameters     811
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.0933
_refine_ls_R_factor_gt           0.0637
_refine_ls_wR_factor_ref         0.1697
_refine_ls_wR_factor_gt          0.1558
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_restrained_S_all      0.994
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ca1 Ca 0.03429(4) 0.36635(4) 0.02429(3) 0.0190(2) Uani 1 1 d . . . . .
Ca2 Ca -0.03439(4) 0.33191(3) 0.13690(3) 0.0188(2) Uani 1 1 d . . . . .
Ca3 Ca -0.05723(4) 0.33342(4) -0.08610(4) 0.0215(2) Uani 1 1 d . . . . .
C1A C 0.0232(3) 0.4537(2) -0.0284(2) 0.0402(14) Uani 1 1 d . . . . .
C1B C 0.09125(17) 0.41014(17) 0.13290(16) 0.0200(9) Uani 1 1 d . . . . .
C1C C -0.09115(18) 0.31913(18) 0.02833(17) 0.0213(10) Uani 1 1 d . . . . .
C1D C 0.0001(2) 0.25278(19) 0.08074(19) 0.0287(11) Uani 1 1 d . . . . .
C1S C -0.1782(4) 0.3388(4) -0.0847(3) 0.081(2) Uani 1 1 d D U . . .
H1S H -0.2059 0.3061 -0.0962 0.098 Uiso 1 1 calc R U . . .
C1T C -0.1585(4) 0.2288(4) 0.1307(4) 0.108(4) Uani 1 1 d . . . . .
H1T H -0.1411 0.2118 0.1173 0.129 Uiso 1 1 calc R U . . .
C1U C 0.1238(11) 0.2904(10) 0.1450(7) 0.187(11) Uani 1 1 d . . . . .
H1U H 0.1117 0.3151 0.1431 0.224 Uiso 1 1 calc R U . . .
C1V C 0.1578(3) 0.3857(5) 0.0313(4) 0.122(5) Uani 1 1 d D . . . .
H1V H 0.1419 0.3523 0.0465 0.147 Uiso 1 1 calc R U . . .
C2A C 0.0297(2) 0.50685(18) -0.04377(18) 0.0326(12) Uani 1 1 d . . . . .
C2B C 0.14313(17) 0.46125(18) 0.12139(16) 0.0218(9) Uani 1 1 d . . . . .
C2C C -0.14333(17) 0.31790(18) 0.03948(16) 0.0193(9) Uani 1 1 d . . . . .
C2D C -0.0002(2) 0.19908(19) 0.08101(18) 0.0283(11) Uani 1 1 d . . . . .
C2T C -0.2374(5) 0.2234(7) 0.1576(6) 0.185(10) Uani 1 1 d . . . . .
H2T1 H -0.2114 0.2529 0.1764 0.277 Uiso 1 1 d R U . . .
H2T2 H -0.2644 0.1964 0.1778 0.277 Uiso 1 1 d R U . . .
H2T3 H -0.2543 0.2363 0.1360 0.277 Uiso 1 1 d R U . . .
C2U C 0.1141(5) 0.2065(6) 0.1736(4) 0.129(5) Uani 1 1 d . . . . .
H2U1 H 0.1475 0.2195 0.1566 0.193 Uiso 1 1 d R U . . .
H2U2 H 0.0870 0.1732 0.1598 0.193 Uiso 1 1 d R U . . .
H2U3 H 0.1195 0.2004 0.2060 0.193 Uiso 1 1 d R U . . .
C3A C -0.0041(2) 0.5085(2) -0.0764(2) 0.0480(16) Uani 1 1 d . . . . .
H3A H -0.0295 0.4766 -0.0909 0.058 Uiso 1 1 calc R U . . .
C3B C 0.14426(18) 0.49908(18) 0.09033(17) 0.0250(10) Uani 1 1 d . . . . .
H3B H 0.1130 0.4915 0.0739 0.030 Uiso 1 1 calc R U . . .
C3C C -0.14430(18) 0.35489(18) 0.07085(17) 0.0220(9) Uani 1 1 d . . . . .
H3C H -0.1132 0.3781 0.0876 0.026 Uiso 1 1 calc R U . . .
C3D C -0.0398(2) 0.1551(2) 0.10238(19) 0.0307(11) Uani 1 1 d . . . . .
H3D H -0.0675 0.1578 0.1170 0.037 Uiso 1 1 calc R U . . .
C3T C -0.2453(6) 0.1463(7) 0.1142(7) 0.216(10) Uani 1 1 d . . . . .
H3T1 H -0.2305 0.1350 0.0891 0.325 Uiso 1 1 d R U . . .
H3T2 H -0.2776 0.1454 0.1033 0.325 Uiso 1 1 d R U . . .
H3T3 H -0.2540 0.1221 0.1406 0.325 Uiso 1 1 d R U . . .
C3U C 0.0545(7) 0.2412(8) 0.1928(5) 0.200(10) Uani 1 1 d . . . . .
H3U1 H 0.0634 0.2715 0.2131 0.301 Uiso 1 1 d R U . . .
H3U2 H 0.0400 0.2088 0.2114 0.301 Uiso 1 1 d R U . . .
H3U3 H 0.0281 0.2379 0.1700 0.301 Uiso 1 1 d R U . . .
C3V C 0.2456(5) 0.3915(10) 0.0443(6) 0.230(12) Uani 1 1 d . . . . .
H3V1 H 0.2255 0.3531 0.0503 0.344 Uiso 1 1 d R U . . .
H3V2 H 0.2637 0.4100 0.0729 0.344 Uiso 1 1 d R U . . .
H3V3 H 0.2724 0.3988 0.0203 0.344 Uiso 1 1 d R U . . .
C4A C -0.0020(3) 0.5565(2) -0.0888(3) 0.061(2) Uani 1 1 d . . . . .
H4A H -0.0267 0.5562 -0.1103 0.074 Uiso 1 1 calc R U . . .
C4B C 0.19135(18) 0.54850(18) 0.08312(18) 0.0245(10) Uani 1 1 d . . . . .
H4B H 0.1915 0.5737 0.0622 0.029 Uiso 1 1 calc R U . . .
C4C C -0.19087(18) 0.35783(18) 0.07751(18) 0.0252(10) Uani 1 1 d . . . . .
H4C H -0.1907 0.3834 0.0980 0.030 Uiso 1 1 calc R U . . .
C4D C -0.0414(2) 0.10590(19) 0.1037(2) 0.0318(12) Uani 1 1 d . . . . .
H4D H -0.0690 0.0765 0.1195 0.038 Uiso 1 1 calc R U . . .
C5A C 0.0367(2) 0.6045(2) -0.0691(2) 0.0413(15) Uani 1 1 d . . . . .
C5B C 0.23837(16) 0.55977(16) 0.10763(16) 0.0185(9) Uani 1 1 d . . . . .
C5C C -0.23821(17) 0.32199(17) 0.05323(16) 0.0200(9) Uani 1 1 d . . . . .
C5D C 0.0002(2) 0.10131(17) 0.08017(19) 0.0262(10) Uani 1 1 d . . . . .
C6A C 0.0727(2) 0.6035(2) -0.0359(2) 0.0384(14) Uani 1 1 d . . . . .
H6A H 0.0990 0.6355 -0.0222 0.046 Uiso 1 1 calc R U . . .
C6B C 0.23780(17) 0.52086(17) 0.13739(17) 0.0225(10) Uani 1 1 d . . . . .
H6B H 0.2693 0.5276 0.1529 0.027 Uiso 1 1 calc R U . . .
C6C C -0.23815(18) 0.28336(18) 0.02386(17) 0.0221(9) Uani 1 1 d . . . . .
H6C H -0.2699 0.2584 0.0087 0.026 Uiso 1 1 calc R U . . .
C6D C 0.0414(2) 0.14715(19) 0.0574(2) 0.0301(11) Uani 1 1 d . . . . .
H6D H 0.0694 0.1452 0.0424 0.036 Uiso 1 1 calc R U . . .
C7A C 0.0691(2) 0.5545(2) -0.0233(2) 0.0355(12) Uani 1 1 d . . . . .
H7A H 0.0930 0.5538 -0.0014 0.043 Uiso 1 1 calc R U . . .
C7B C 0.19041(18) 0.47187(18) 0.14418(17) 0.0229(10) Uani 1 1 d . . . . .
H7B H 0.1904 0.4460 0.1642 0.027 Uiso 1 1 calc R U . . .
C7C C -0.19012(17) 0.28163(18) 0.01677(16) 0.0219(9) Uani 1 1 d . . . . .
H7C H -0.1901 0.2559 -0.0033 0.026 Uiso 1 1 calc R U . . .
C7D C 0.0407(2) 0.1957(2) 0.05728(19) 0.0295(11) Uani 1 1 d . . . . .
H7D H 0.0674 0.2256 0.0414 0.035 Uiso 1 1 calc R U . . .
C8A C 0.0378(2) 0.6565(2) -0.0790(3) 0.0482(18) Uani 1 1 d . . . . .
C8B C 0.28750(17) 0.61487(17) 0.10463(16) 0.0200(9) Uani 1 1 d . . . . .
C8C C -0.28709(17) 0.32780(17) 0.05665(16) 0.0191(9) Uani 1 1 d . . . . .
C8D C -0.00035(18) 0.04888(18) 0.0801(2) 0.0276(11) Uani 1 1 d . . . . .
C9A C -0.0099(2) 0.6562(2) -0.0870(3) 0.0532(18) Uani 1 1 d . . . . .
H9A H -0.0423 0.6235 -0.0880 0.064 Uiso 1 1 calc R U . . .
C9B C 0.28180(17) 0.66045(17) 0.10445(16) 0.0195(9) Uani 1 1 d . . . . .
H9B H 0.2474 0.6564 0.1042 0.023 Uiso 1 1 calc R U . . .
C9C C -0.28205(17) 0.37840(17) 0.05717(16) 0.0201(9) Uani 1 1 d . . . . .
H9C H -0.2477 0.4088 0.0579 0.024 Uiso 1 1 calc R U . . .
C9D C -0.04858(19) 0.00018(19) 0.0806(2) 0.0287(11) Uani 1 1 d . . . . .
H9D H -0.0812 0.0001 0.0812 0.034 Uiso 1 1 calc R U . . .
C10A C 0.0862(2) 0.7053(2) -0.0792(2) 0.0406(14) Uani 1 1 d . . . . .
H10A H 0.1185 0.7054 -0.0745 0.049 Uiso 1 1 calc R U . . .
C11A C -0.0867(2) 0.6175(2) 0.2418(3) 0.0508(18) Uani 1 1 d . . . . .
H11A H -0.1190 0.5849 0.2395 0.061 Uiso 1 1 calc R U . . .
C12A C -0.0382(2) 0.6181(2) 0.2398(3) 0.0470(17) Uani 1 1 d . . . . .
C13A C -0.0363(2) 0.5678(2) 0.2300(3) 0.0482(17) Uani 1 1 d . . . . .
C14A C -0.0726(2) 0.5307(2) 0.1968(2) 0.0397(14) Uani 1 1 d . . . . .
H14A H -0.0989 0.5365 0.1832 0.048 Uiso 1 1 calc R U . . .
C15A C -0.0690(2) 0.4858(2) 0.1844(2) 0.0347(12) Uani 1 1 d . . . . .
H15A H -0.0935 0.4611 0.1628 0.042 Uiso 1 1 calc R U . . .
C16A C -0.0297(2) 0.4772(2) 0.20372(18) 0.0319(12) Uani 1 1 d . . . . .
C17A C 0.0047(3) 0.5130(3) 0.2378(3) 0.0533(17) Uani 1 1 d . . . . .
H17A H 0.0303 0.5069 0.2523 0.064 Uiso 1 1 calc R U . . .
C18A C 0.0006(3) 0.5574(3) 0.2499(3) 0.068(2) Uani 1 1 d . . . . .
H18A H 0.0239 0.5811 0.2726 0.082 Uiso 1 1 calc R U . . .
C19A C -0.0234(3) 0.4298(3) 0.1884(2) 0.0429(15) Uani 1 1 d . . . . .
C20A C 0.24607(19) 0.3335(2) -0.0862(2) 0.0409(15) Uani 1 1 d . . . . .
C21A C 0.19485(19) 0.3341(2) -0.0859(2) 0.0334(12) Uani 1 1 d . . . . .
C22A C 0.15208(19) 0.29841(19) -0.0562(2) 0.0295(11) Uani 1 1 d . . . . .
H22A H 0.1562 0.2745 -0.0366 0.035 Uiso 1 1 calc R U . . .
C23A C 0.1038(2) 0.29919(19) -0.05634(19) 0.0297(11) Uani 1 1 d . . . . .
H23A H 0.0757 0.2762 -0.0364 0.036 Uiso 1 1 calc R U . . .
C24A C 0.09752(16) 0.33432(19) -0.08626(16) 0.0180(9) Uani 1 1 d . . . . .
C25A C 0.13815(19) 0.36742(19) -0.11659(19) 0.0279(11) Uani 1 1 d . . . . .
H25A H 0.1328 0.3892 -0.1378 0.033 Uiso 1 1 calc R U . . .
C26A C 0.1868(2) 0.3684(2) -0.1156(2) 0.0353(13) Uani 1 1 d . . . . .
H26A H 0.2148 0.3925 -0.1350 0.042 Uiso 1 1 calc R U . . .
C27A C 0.04427(16) 0.33361(18) -0.08609(16) 0.0185(9) Uani 1 1 d . . . . .
N1T N -0.2075(4) 0.1991(4) 0.1296(5) 0.164(7) Uani 1 1 d . . . . .
N1U N 0.0979(5) 0.2461(7) 0.1715(5) 0.158(7) Uani 1 1 d . . . . .
N1V N 0.2090(3) 0.4092(5) 0.0288(4) 0.132(5) Uani 1 1 d D . . . .
O1A O -0.0111(3) 0.41158(17) -0.04764(18) 0.0782(18) Uani 1 1 d . . . . .
O1B O 0.05193(13) 0.39493(13) 0.10373(12) 0.0256(7) Uani 1 1 d . . . . .
O1C O -0.08779(13) 0.29790(15) -0.00902(11) 0.0275(7) Uani 1 1 d . . . . .
O1D O -0.03171(16) 0.25643(14) 0.10783(14) 0.0372(9) Uani 1 1 d . . . . .
O1S O -0.1309(4) 0.3448(4) -0.0829(4) 0.156(2) Uani 1 1 d . U . . .
O1T O -0.12709(15) 0.27207(19) 0.14350(16) 0.0503(12) Uani 1 1 d . . . . .
O1U O 0.1646(5) 0.2978(6) 0.1228(4) 0.174(5) Uani 1 1 d . . . . .
O1V O 0.12669(15) 0.39891(17) 0.01767(17) 0.0499(12) Uani 1 1 d . . . . .
O2A O 0.0533(2) 0.45385(18) 0.0032(2) 0.0691(15) Uani 1 1 d . . . . .
O2B O -0.05274(13) 0.36870(14) -0.16335(12) 0.0278(7) Uani 1 1 d . . . . .
O2C O -0.05153(12) 0.34414(13) 0.05729(12) 0.0226(7) Uani 1 1 d . . . . .
O2D O 0.03193(16) 0.28837(14) 0.05349(13) 0.0357(9) Uani 1 1 d . . . . .
O3A O -0.0526(2) 0.4005(2) 0.1579(2) 0.0723(16) Uani 1 1 d . . . . .
O4A O 0.0102(3) 0.4216(2) 0.20827(18) 0.0820(19) Uani 1 1 d . . . . .
O5A O 0.01754(13) 0.32247(13) -0.04837(11) 0.0220(7) Uani 1 1 d . . . . .
O6A O -0.01755(13) 0.30474(12) 0.20928(11) 0.0232(7) Uani 1 1 d . . . . .
N1S N -0.1916(4) 0.3768(5) -0.0709(3) 0.114(3) Uani 1 1 d D . . . .
C2S C -0.1528(10) 0.4295(7) -0.0509(8) 0.306(16) Uani 1 1 d D . . . .
H2S1 H -0.1317 0.4302 -0.0187 0.459 Uiso 1 1 d R U . . .
H2S2 H -0.1662 0.4582 -0.0386 0.459 Uiso 1 1 d R U . . .
H2S3 H -0.1168 0.4598 -0.0703 0.459 Uiso 1 1 d R U . . .
C3S C -0.2532(6) 0.3487(9) -0.0792(6) 0.194(10) Uani 1 1 d D . . . .
H3S1 H -0.2705 0.3114 -0.0930 0.291 Uiso 1 1 d R U . . .
H3S2 H -0.2642 0.3697 -0.1004 0.291 Uiso 1 1 d R U . . .
H3S3 H -0.2727 0.3447 -0.0487 0.291 Uiso 1 1 d R U . . .
C2V C 0.2335(8) 0.4622(7) 0.0065(7) 0.204(9) Uani 1 1 d D . . . .
H2V1 H 0.2491 0.4604 -0.0231 0.306 Uiso 1 1 d R U . . .
H2V2 H 0.2614 0.4883 0.0266 0.306 Uiso 1 1 d R U . . .
H2V3 H 0.2070 0.4729 0.0008 0.306 Uiso 1 1 d R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ca1 O1V 2.325(4) . ?
Ca1 O5A 2.330(3) . ?
Ca1 O2D 2.344(3) . ?
Ca1 O2A 2.353(4) . ?
Ca1 O1B 2.359(3) . ?
Ca1 O2C 2.393(3) . ?
Ca1 O1A 3.028(6) . ?
Ca1 C1A 3.056(6) . ?
Ca1 C1C 3.135(4) . ?
Ca1 Ca2 3.6119(11) . ?
Ca1 Ca3 3.8755(13) . ?
Ca2 O6A 2.325(3) . ?
Ca2 O1T 2.332(4) . ?
Ca2 O3A 2.342(4) . ?
Ca2 O1D 2.344(3) . ?
Ca2 O2C 2.369(3) . ?
Ca2 O1B 2.400(3) . ?
Ca2 O4A 2.999(6) . ?
Ca2 C19A 3.027(6) . ?
Ca2 C1B 3.140(4) . ?
Ca2 Ca3 3.8770(13) 6_455 ?
Ca3 O1A 2.227(5) . ?
Ca3 O4A 2.236(5) 8_554 ?
Ca3 O1S 2.286(11) . ?
Ca3 O1C 2.380(3) . ?
Ca3 O2B 2.384(3) . ?
Ca3 O5A 2.542(3) . ?
Ca3 O6A 2.548(3) 8_554 ?
Ca3 C27A 2.895(4) . ?
Ca3 Ca2 3.8771(13) 8_554 ?
C1A O1A 1.235(7) . ?
C1A O2A 1.240(8) . ?
C1A C2A 1.498(7) . ?
C1C O1C 1.246(6) . ?
C1C O2C 1.286(6) . ?
C1C C2C 1.506(6) . ?
C1D O1D 1.232(7) . ?
C1D O2D 1.237(7) . ?
C1D C2D 1.529(6) . ?
C1B O2B 1.233(6) 6_455 ?
C1B O1B 1.282(6) . ?
C1B C2B 1.506(6) . ?
C1S O1S 1.274(12) . ?
C1S N1S 1.377(12) . ?
C1T O1T 1.164(11) . ?
C1T N1T 1.221(11) . ?
C1U O1U 1.24(2) . ?
C1U N1U 1.33(3) . ?
C1V O1V 1.191(11) . ?
C1V N1V 1.268(11) . ?
C2A C3A 1.356(8) . ?
C2A C7A 1.386(7) . ?
C2C C7C 1.374(6) . ?
C2C C3C 1.391(6) . ?
C2D C3D 1.342(8) . ?
C2D C7D 1.392(7) . ?
C2B C3B 1.381(7) . ?
C2B C7B 1.386(6) . ?
C2T N1T 1.56(2) . ?
C2U N1U 1.423(14) . ?
C3A C4A 1.385(9) . ?
C3C C4C 1.386(6) . ?
C3D C4D 1.383(7) . ?
C3B C4B 1.394(6) . ?
C3T N1T 1.413(18) . ?
C3U N1U 1.320(19) . ?
C3V N1V 1.441(18) . ?
C4A C5A 1.377(8) . ?
C4C C5C 1.401(7) . ?
C4D C5D 1.422(7) . ?
C4B C5B 1.398(6) . ?
C5A C6A 1.405(7) . ?
C5A C8A 1.494(7) . ?
C5C C6C 1.382(6) . ?
C5C C8C 1.489(6) . ?
C5D C6D 1.405(7) . ?
C5D C8D 1.490(6) . ?
C5B C6B 1.388(6) . ?
C5B C8B 1.498(6) . ?
C6A C7A 1.397(7) . ?
C6C C7C 1.411(6) . ?
C6D C7D 1.397(7) . ?
C6B C7B 1.390(6) . ?
C8A C9A 1.378(8) . ?
C8A C10A 1.386(7) . ?
C8C C9C 1.379(6) . ?
C8C C9C 1.412(6) 3_455 ?
C8D C9D 1.384(7) . ?
C8D C9D 1.407(6) 3 ?
C8B C9B 1.390(6) . ?
C8B C9B 1.403(6) 2_665 ?
C9A C12A 1.407(8) 9_454 ?
C9C C8C 1.412(6) 2_565 ?
C9D C8D 1.407(6) 2 ?
C9B C8B 1.403(6) 3_565 ?
C10A C20A 1.386(7) 3_565 ?
C11A C12A 1.377(7) . ?
C11A C20A 1.424(7) 4_455 ?
C12A C9A 1.408(8) 5_565 ?
C12A C13A 1.489(7) . ?
C13A C18A 1.353(8) . ?
C13A C14A 1.406(8) . ?
C14A C15A 1.383(7) . ?
C15A C16A 1.377(7) . ?
C16A C17A 1.391(8) . ?
C16A C19A 1.515(7) . ?
C17A C18A 1.372(9) . ?
C19A O3A 1.203(8) . ?
C19A O4A 1.232(8) . ?
C20A C10A 1.386(7) 2_665 ?
C20A C11A 1.424(7) 7_544 ?
C20A C21A 1.471(6) . ?
C21A C26A 1.396(8) . ?
C21A C22A 1.411(8) . ?
C22A C23A 1.390(7) . ?
C23A C24A 1.391(7) . ?
C24A C25A 1.371(7) . ?
C24A C27A 1.510(5) . ?
C25A C26A 1.375(7) . ?
C27A O5A 1.257(5) . ?
C27A O6A 1.260(5) 8_554 ?
N1V C2V 1.455(16) . ?
O2B C1B 1.233(6) 8_554 ?
O4A Ca3 2.235(5) 6_455 ?
O6A C27A 1.260(5) 6_455 ?
O6A Ca3 2.547(3) 6_455 ?
N1S C2S 1.464(17) . ?
N1S C3S 1.543(15) . ?

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
O1V Ca1 O5A 91.76(13) . . ?
O1V Ca1 O2D 84.04(16) . . ?
O5A Ca1 O2D 84.26(12) . . ?
O1V Ca1 O2A 86.65(18) . . ?
O5A Ca1 O2A 102.91(17) . . ?
O2D Ca1 O2A 168.44(17) . . ?
O1V Ca1 O1B 86.28(14) . . ?
O5A Ca1 O1B 168.04(12) . . ?
O2D Ca1 O1B 83.80(13) . . ?
O2A Ca1 O1B 88.77(17) . . ?
O1V Ca1 O2C 160.77(14) . . ?
O5A Ca1 O2C 107.13(11) . . ?
O2D Ca1 O2C 94.09(13) . . ?
O2A Ca1 O2C 92.45(16) . . ?
O1B Ca1 O2C 74.50(11) . . ?
O1V Ca1 O1A 114.68(18) . . ?
O5A Ca1 O1A 67.62(12) . . ?
O2D Ca1 O1A 145.80(13) . . ?
O2A Ca1 O1A 45.36(16) . . ?
O1B Ca1 O1A 123.80(13) . . ?
O2C Ca1 O1A 77.02(14) . . ?
O1V Ca1 C1A 101.20(18) . . ?
O5A Ca1 C1A 86.04(13) . . ?
O2D Ca1 C1A 169.11(16) . . ?
O2A Ca1 C1A 21.96(17) . . ?
O1B Ca1 C1A 105.92(14) . . ?
O2C Ca1 C1A 84.06(14) . . ?
O1A Ca1 C1A 23.42(14) . . ?
O1V Ca1 C1C 177.04(14) . . ?
O5A Ca1 C1C 85.29(12) . . ?
O2D Ca1 C1C 95.42(13) . . ?
O2A Ca1 C1C 94.22(16) . . ?
O1B Ca1 C1C 96.57(12) . . ?
O2C Ca1 C1C 22.10(12) . . ?
O1A Ca1 C1C 64.35(14) . . ?
C1A Ca1 C1C 78.84(14) . . ?
O1V Ca1 Ca2 122.20(12) . . ?
O5A Ca1 Ca2 134.04(9) . . ?
O2D Ca1 Ca2 71.11(10) . . ?
O2A Ca1 Ca2 108.58(15) . . ?
O1B Ca1 Ca2 41.05(8) . . ?
O2C Ca1 Ca2 40.41(8) . . ?
O1A Ca1 Ca2 114.80(12) . . ?
C1A Ca1 Ca2 112.91(11) . . ?
C1C Ca1 Ca2 60.18(9) . . ?
O1V Ca1 Ca3 121.64(12) . . ?
O5A Ca1 Ca3 39.25(8) . . ?
O2D Ca1 Ca3 110.99(10) . . ?
O2A Ca1 Ca3 79.79(14) . . ?
O1B Ca1 Ca3 148.65(9) . . ?
O2C Ca1 Ca3 76.92(8) . . ?
O1A Ca1 Ca3 34.99(8) . . ?
C1A Ca1 Ca3 58.13(12) . . ?
C1C Ca1 Ca3 55.84(9) . . ?
Ca2 Ca1 Ca3 115.92(3) . . ?
O6A Ca2 O1T 91.90(13) . . ?
O6A Ca2 O3A 103.03(18) . . ?
O1T Ca2 O3A 86.95(18) . . ?
O6A Ca2 O1D 83.99(13) . . ?
O1T Ca2 O1D 84.34(16) . . ?
O3A Ca2 O1D 169.00(17) . . ?
O6A Ca2 O2C 168.57(12) . . ?
O1T Ca2 O2C 86.66(13) . . ?
O3A Ca2 O2C 88.22(17) . . ?
O1D Ca2 O2C 84.59(13) . . ?
O6A Ca2 O1B 106.79(12) . . ?
O1T Ca2 O1B 160.86(14) . . ?
O3A Ca2 O1B 92.68(17) . . ?
O1D Ca2 O1B 93.36(13) . . ?
O2C Ca2 O1B 74.20(11) . . ?
O6A Ca2 O4A 67.70(12) . . ?
O1T Ca2 O4A 114.42(18) . . ?
O3A Ca2 O4A 44.97(16) . . ?
O1D Ca2 O4A 145.69(13) . . ?
O2C Ca2 O4A 123.10(13) . . ?
O1B Ca2 O4A 77.59(15) . . ?
O6A Ca2 C19A 86.56(13) . . ?
O1T Ca2 C19A 101.16(18) . . ?
O3A Ca2 C19A 21.40(17) . . ?
O1D Ca2 C19A 169.23(16) . . ?
O2C Ca2 C19A 104.84(13) . . ?
O1B Ca2 C19A 84.42(15) . . ?
O4A Ca2 C19A 23.59(15) . . ?
O6A Ca2 C1B 85.17(12) . . ?
O1T Ca2 C1B 177.07(14) . . ?
O3A Ca2 C1B 93.85(16) . . ?
O1D Ca2 C1B 95.19(13) . . ?
O2C Ca2 C1B 96.18(12) . . ?
O1B Ca2 C1B 21.98(12) . . ?
O4A Ca2 C1B 64.57(14) . . ?
C19A Ca2 C1B 78.84(15) . . ?
O6A Ca2 Ca1 133.95(9) . . ?
O1T Ca2 Ca1 122.21(12) . . ?
O3A Ca2 Ca1 108.28(16) . . ?
O1D Ca2 Ca1 71.19(10) . . ?
O2C Ca2 Ca1 40.91(7) . . ?
O1B Ca2 Ca1 40.21(8) . . ?
O4A Ca2 Ca1 114.91(12) . . ?
C19A Ca2 Ca1 112.49(11) . . ?
C1B Ca2 Ca1 60.19(9) . . ?
O6A Ca2 Ca3 39.32(8) . 6_455 ?
O1T Ca2 Ca3 121.73(12) . 6_455 ?
O3A Ca2 Ca3 79.58(14) . 6_455 ?
O1D Ca2 Ca3 110.76(10) . 6_455 ?
O2C Ca2 Ca3 147.94(8) . 6_455 ?
O1B Ca2 Ca3 76.87(8) . 6_455 ?
O4A Ca2 Ca3 35.09(9) . 6_455 ?
C19A Ca2 Ca3 58.47(12) . 6_455 ?
C1B Ca2 Ca3 55.75(9) . 6_455 ?
Ca1 Ca2 Ca3 115.85(3) . 6_455 ?
O1A Ca3 O4A 168.9(3) . 8_554 ?
O1A Ca3 O1S 87.9(3) . . ?
O4A Ca3 O1S 103.1(3) 8_554 . ?
O1A Ca3 O1C 83.44(16) . . ?
O4A Ca3 O1C 98.59(16) 8_554 . ?
O1S Ca3 O1C 81.8(3) . . ?
O1A Ca3 O2B 98.33(16) . . ?
O4A Ca3 O2B 83.10(15) 8_554 . ?
O1S Ca3 O2B 80.5(3) . . ?
O1C Ca3 O2B 162.10(11) . . ?
O1A Ca3 O5A 78.82(19) . . ?
O4A Ca3 O5A 91.30(19) 8_554 . ?
O1S Ca3 O5A 152.9(3) . . ?
O1C Ca3 O5A 73.39(11) . . ?
O2B Ca3 O5A 124.49(11) . . ?
O1A Ca3 O6A 91.89(19) . 8_554 ?
O4A Ca3 O6A 77.95(19) 8_554 8_554 ?
O1S Ca3 O6A 153.7(3) . 8_554 ?
O1C Ca3 O6A 124.35(11) . 8_554 ?
O2B Ca3 O6A 73.51(11) . 8_554 ?
O5A Ca3 O6A 51.47(9) . 8_554 ?
O1A Ca3 C27A 84.8(2) . . ?
O4A Ca3 C27A 84.2(2) 8_554 . ?
O1S Ca3 C27A 172.5(3) . . ?
O1C Ca3 C27A 98.87(12) . . ?
O2B Ca3 C27A 99.03(12) . . ?
O5A Ca3 C27A 25.70(12) . . ?
O6A Ca3 C27A 25.76(12) 8_554 . ?
O1A Ca3 Ca1 51.24(15) . . ?
O4A Ca3 Ca1 121.49(16) 8_554 . ?
O1S Ca3 Ca1 119.4(3) . . ?
O1C Ca3 Ca1 54.78(8) . . ?
O2B Ca3 Ca1 138.57(9) . . ?
O5A Ca3 Ca1 35.45(7) . . ?
O6A Ca3 Ca1 79.62(7) 8_554 . ?
C27A Ca3 Ca1 56.41(9) . . ?
O1A Ca3 Ca2 121.80(16) . 8_554 ?
O4A Ca3 Ca2 50.47(15) 8_554 8_554 ?
O1S Ca3 Ca2 127.3(3) . 8_554 ?
O1C Ca3 Ca2 138.23(9) . 8_554 ?
O2B Ca3 Ca2 54.93(8) . 8_554 ?
O5A Ca3 Ca2 79.46(7) . 8_554 ?
O6A Ca3 Ca2 35.32(7) 8_554 8_554 ?
C27A Ca3 Ca2 56.41(9) . 8_554 ?
Ca1 Ca3 Ca2 112.82(3) . 8_554 ?
O1A C1A O2A 122.2(5) . . ?
O1A C1A C2A 119.7(6) . . ?
O2A C1A C2A 118.1(5) . . ?
O1A C1A Ca1 77.0(3) . . ?
O2A C1A Ca1 45.2(3) . . ?
C2A C1A Ca1 163.2(4) . . ?
O1C C1C O2C 123.4(4) . . ?
O1C C1C C2C 118.8(4) . . ?
O2C C1C C2C 117.7(4) . . ?
O1C C1C Ca1 80.2(3) . . ?
O2C C1C Ca1 44.4(2) . . ?
C2C C1C Ca1 157.2(3) . . ?
O1D C1D O2D 126.1(4) . . ?
O1D C1D C2D 116.5(5) . . ?
O2D C1D C2D 117.4(5) . . ?
O2B C1B O1B 123.5(4) 6_455 . ?
O2B C1B C2B 119.1(4) 6_455 . ?
O1B C1B C2B 117.4(4) . . ?
O2B C1B Ca2 80.4(3) 6_455 . ?
O1B C1B Ca2 44.5(2) . . ?
C2B C1B Ca2 156.6(3) . . ?
O1S C1S N1S 125.3(10) . . ?
O1T C1T N1T 138.7(16) . . ?
O1U C1U N1U 118.4(17) . . ?
O1V C1V N1V 131.1(14) . . ?
C3A C2A C7A 119.6(5) . . ?
C3A C2A C1A 120.2(5) . . ?
C7A C2A C1A 120.1(5) . . ?
C7C C2C C3C 119.4(4) . . ?
C7C C2C C1C 119.8(4) . . ?
C3C C2C C1C 120.7(4) . . ?
C3D C2D C7D 119.7(4) . . ?
C3D C2D C1D 121.4(5) . . ?
C7D C2D C1D 118.9(5) . . ?
C3B C2B C7B 119.1(4) . . ?
C3B C2B C1B 121.5(4) . . ?
C7B C2B C1B 119.3(4) . . ?
C2A C3A C4A 121.8(5) . . ?
C4C C3C C2C 121.1(4) . . ?
C2D C3D C4D 123.2(5) . . ?
C2B C3B C4B 121.2(4) . . ?
C5A C4A C3A 120.0(6) . . ?
C3C C4C C5C 119.6(4) . . ?
C3D C4D C5D 118.4(5) . . ?
C3B C4B C5B 119.3(4) . . ?
C4A C5A C6A 118.7(5) . . ?
C4A C5A C8A 121.5(5) . . ?
C6A C5A C8A 119.6(5) . . ?
C6C C5C C4C 119.5(4) . . ?
C6C C5C C8C 120.2(4) . . ?
C4C C5C C8C 120.2(4) . . ?
C6D C5D C4D 118.6(4) . . ?
C6D C5D C8D 121.2(4) . . ?
C4D C5D C8D 120.2(4) . . ?
C6B C5B C4B 119.4(4) . . ?
C6B C5B C8B 120.4(4) . . ?
C4B C5B C8B 120.0(4) . . ?
C7A C6A C5A 120.3(5) . . ?
C5C C6C C7C 120.2(4) . . ?
C7D C6D C5D 120.3(5) . . ?
C5B C6B C7B 120.4(4) . . ?
C2A C7A C6A 119.6(5) . . ?
C2C C7C C6C 120.2(4) . . ?
C2D C7D C6D 119.8(5) . . ?
C2B C7B C6B 120.5(4) . . ?
C9A C8A C10A 119.4(5) . . ?
C9A C8A C5A 119.6(4) . . ?
C10A C8A C5A 121.0(5) . . ?
C9C C8C C9C 118.4(4) . 3_455 ?
C9C C8C C5C 120.3(4) . . ?
C9C C8C C5C 121.2(4) 3_455 . ?
C9D C8D C9D 119.2(5) . 3 ?
C9D C8D C5D 121.0(4) . . ?
C9D C8D C5D 119.8(4) 3 . ?
C9B C8B C9B 119.2(4) . 2_665 ?
C9B C8B C5B 119.8(4) . . ?
C9B C8B C5B 120.9(4) 2_665 . ?
C8A C9A C12A 120.9(5) . 9_454 ?
C8C C9C C8C 121.5(4) . 2_565 ?
C8D C9D C8D 120.8(5) . 2 ?
C8B C9B C8B 120.7(4) . 3_565 ?
C8A C10A C20A 121.4(5) . 3_565 ?
C12A C11A C20A 120.1(5) . 4_455 ?
C11A C12A C9A 119.4(5) . 5_565 ?
C11A C12A C13A 121.1(5) . . ?
C9A C12A C13A 119.5(5) 5_565 . ?
C18A C13A C14A 118.3(5) . . ?
C18A C13A C12A 122.8(5) . . ?
C14A C13A C12A 118.8(5) . . ?
C15A C14A C13A 120.0(5) . . ?
C16A C15A C14A 120.6(5) . . ?
C15A C16A C17A 118.9(4) . . ?
C15A C16A C19A 121.1(5) . . ?
C17A C16A C19A 120.0(5) . . ?
C18A C17A C16A 119.8(5) . . ?
C13A C18A C17A 122.3(6) . . ?
O3A C19A O4A 122.1(6) . . ?
O3A C19A C16A 118.4(5) . . ?
O4A C19A C16A 119.5(6) . . ?
O3A C19A Ca2 45.3(3) . . ?
O4A C19A Ca2 76.9(4) . . ?
C16A C19A Ca2 163.5(4) . . ?
C10A C20A C11A 118.6(4) 2_665 7_544 ?
C10A C20A C21A 120.3(5) 2_665 . ?
C11A C20A C21A 121.0(4) 7_544 . ?
C26A C21A C22A 118.6(4) . . ?
C26A C21A C20A 121.3(5) . . ?
C22A C21A C20A 120.1(5) . . ?
C23A C22A C21A 119.6(5) . . ?
C24A C23A C22A 120.0(5) . . ?
C25A C24A C23A 120.6(4) . . ?
C25A C24A C27A 120.7(4) . . ?
C23A C24A C27A 118.7(4) . . ?
C24A C25A C26A 120.0(5) . . ?
C25A C26A C21A 121.1(5) . . ?
O5A C27A O6A 122.8(4) . 8_554 ?
O5A C27A C24A 119.1(4) . . ?
O6A C27A C24A 118.2(4) 8_554 . ?
O5A C27A Ca3 61.3(2) . . ?
O6A C27A Ca3 61.5(2) 8_554 . ?
C24A C27A Ca3 179.4(3) . . ?
C1T N1T C3T 138.3(19) . . ?
C1T N1T C2T 111.8(14) . . ?
C3T N1T C2T 109.5(12) . . ?
C3U N1U C1U 113.9(16) . . ?
C3U N1U C2U 123.9(19) . . ?
C1U N1U C2U 122.1(16) . . ?
C1V N1V C3V 130.0(16) . . ?
C1V N1V C2V 113.9(13) . . ?
C3V N1V C2V 116.2(14) . . ?
C1A O1A Ca3 167.2(6) . . ?
C1A O1A Ca1 79.5(4) . . ?
Ca3 O1A Ca1 93.77(16) . . ?
C1C O1C Ca3 132.2(3) . . ?
C1D O1D Ca2 131.3(3) . . ?
C1B O1B Ca1 136.9(3) . . ?
C1B O1B Ca2 113.5(3) . . ?
Ca1 O1B Ca2 98.74(12) . . ?
C1S O1S Ca3 165.6(9) . . ?
C1T O1T Ca2 137.9(7) . . ?
C1V O1V Ca1 136.4(7) . . ?
C1A O2A Ca1 112.8(4) . . ?
C1C O2C Ca2 135.6(3) . . ?
C1C O2C Ca1 113.5(3) . . ?
Ca2 O2C Ca1 98.68(11) . . ?
C1D O2D Ca1 131.3(3) . . ?
C1B O2B Ca3 132.6(3) 8_554 . ?
C19A O3A Ca2 113.3(4) . . ?
C19A O4A Ca3 168.7(6) . 6_455 ?
C19A O4A Ca2 79.5(4) . . ?
Ca3 O4A Ca2 94.44(15) 6_455 . ?
C27A O5A Ca1 132.7(3) . . ?
C27A O5A Ca3 93.0(2) . . ?
Ca1 O5A Ca3 105.30(11) . . ?
C27A O6A Ca2 133.1(3) 6_455 . ?
C27A O6A Ca3 92.7(3) 6_455 6_455 ?
Ca2 O6A Ca3 105.36(12) . 6_455 ?
C1S N1S C2S 123.6(14) . . ?
C1S N1S C3S 103.9(11) . . ?
C2S N1S C3S 132.4(15) . . ?

_refine_diff_density_max         1.923
_refine_diff_density_min         -0.642
_refine_diff_density_rms         0.069

_shelxl_version_number           2014-3




# start Validation Reply Form
_vrf_CHEMW03_Compound1           
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: Crystal structure of this compound contains many disordered DMF 
molecules occupying the voids. In spite of all efforts to refine them, almost
no residual peaks were found in the Fourier difference, so SQUEEZE routine was
applied and the corresponding hkl file was employed during the last cycles of 
the refinement.
;
_vrf_PLAT220_Compound1           
;
PROBLEM: Non-Solvent Resd 1   C   Ueq(max)/Ueq(min) Range       10.0 Ratio 
RESPONSE: Some coordinated DMF molecules show relatively high anisotropic
displacement parameters owing to the vast disorder present in the voids of
the structure.
;
_vrf_PLAT241_Compound1           
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of        O1S Check 
RESPONSE: Some coordinated DMF molecules show relatively high anisotropic
displacement parameters owing to the vast disorder present in the voids of
the structure.
;
_vrf_PLAT242_Compound1           
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        N1S Check 
RESPONSE: Some coordinated DMF molecules show relatively high anisotropic
displacement parameters owing to the vast disorder present in the voids of
the structure.
;
_vrf_PLAT390_Compound1           
;
PROBLEM: Deviating Methyl C2S     X-C-H Bond Angle ......        121 Degree
RESPONSE: This atom belongs to a DMF molecule affected by the disorder present
in the voids of the structure. Some restraints have been employed to fix the 
positions of some atoms, which makes their hydrogen atoms out of the usual 
parameteres.
;
_vrf_PLAT391_Compound1           
;
PROBLEM: Deviating Methyl C2S     H-C-H Bond Angle ......         97 Degree
RESPONSE: This atom belongs to a DMF molecule affected by the disorder present
in the voids of the structure. Some restraints have been employed to fix the 
positions of some atoms, which makes their hydrogen atoms out of the usual 
parameteres.
;
# end Validation Reply Form

_exptl_crystal_preparation       Luminescent
####################################################################### 
# 
# 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_Compound3
_database_code_depnum_ccdc_archive 'CCDC 1583253'
_audit_update_record             
;
2018-03-28 deposited with the CCDC.
2018-07-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014

_chemical_name_systematic        
"poly-[(mu5-2-amino-1,4-benzenedicarboxylate -kO:k2O,O':kO':k2O'',O''':kO'')(dimethylformamide)barium(II)]"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C11 H12 Ba N2 O5'
_chemical_formula_sum            'C11 H12 Ba N2 O5'
_chemical_formula_weight         389.57

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'
Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           144
_space_group_name_H-M_alt        'P 31'
_space_group_name_Hall           'P 31'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   10.8141(12)
_cell_length_b                   10.8141(12)
_cell_length_c                   10.244(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1037.4(3)
_cell_formula_units_Z            3
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6621
_cell_measurement_theta_min      2.175
_cell_measurement_theta_max      28.339


_exptl_crystal_description       prismatic
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.871
_exptl_crystal_density_method    none
_exptl_crystal_F_000             564
_exptl_absorpt_coefficient_mu    2.888
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
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)
;
_exptl_absorpt_correction_T_min  0.620
_exptl_absorpt_correction_T_max  0.760

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Venture'
_diffrn_measurement_method       ω
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            6621
_diffrn_reflns_av_unetI/netI     0.0571
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.175
_diffrn_reflns_theta_max         28.339
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.941
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.941
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.941
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2629
_reflns_number_gt                2505
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_max     0.941
_reflns_Friedel_fraction_full    1.000

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 Refined as a 2-component inversion twin.
Additionally, the ccordinated DMF molecule is disordered into two 
coplanar disposiitions, which has been modelled by refining three of
its five non-hydrogen atoms into two equivalent positions with 
a 50% of occupation and using some few restraints. 
Although these atoms may be refined with anisotropic
displacement parameters, they acquire somewhat elongated shapes causing
serious alerts. Therefore, the whole DMF molecule has been refined with
isotropic occupancies.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0361P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.02(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2629
_refine_ls_number_parameters     170
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0359
_refine_ls_wR_factor_ref         0.0759
_refine_ls_wR_factor_gt          0.0740
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ba1 Ba 1.77107(5) 1.30667(5) 0.35401(8) 0.01325(13) Uani 1 1 d . . . . .
C1 C 1.5094(9) 1.1285(10) 0.6483(9) 0.0181(19) Uani 1 1 d . . . . .
C2 C 1.3833(10) 0.9888(10) 0.6031(9) 0.0177(18) Uani 1 1 d . . . . .
C3 C 1.3800(10) 0.9402(11) 0.4794(9) 0.031(2) Uani 1 1 d . . . . .
H3 H 1.4585 0.9920 0.4254 0.037 Uiso 1 1 calc R U . . .
C4 C 1.2632(11) 0.8151(11) 0.4306(10) 0.035(3) Uani 1 1 d . . . . .
C5 C 1.1469(9) 0.7377(9) 0.5120(9) 0.0204(19) Uani 1 1 d . . . . .
C6 C 1.1488(11) 0.7905(11) 0.6354(10) 0.032(3) Uani 1 1 d . . . . .
H6 H 1.0690 0.7409 0.6884 0.039 Uiso 1 1 calc R U . . .
C7 C 1.2655(11) 0.9153(11) 0.6839(10) 0.031(2) Uani 1 1 d . . . . .
H7 H 1.2642 0.9479 0.7676 0.037 Uiso 1 1 calc R U . . .
C8 C 1.0208(10) 0.5990(10) 0.4691(9) 0.023(2) Uani 1 1 d . . . . .
N1 N 1.2668(13) 0.7758(14) 0.3060(11) 0.109(7) Uani 1 1 d . . . . .
H1A H 1.1951 0.7003 0.2744 0.131 Uiso 1 1 calc R U . . .
H1B H 1.3407 0.8264 0.2583 0.131 Uiso 1 1 calc R U . . .
O1 O 1.6098(6) 1.1977(6) 0.5678(6) 0.0189(13) Uani 1 1 d . . . . .
O2 O 1.5115(6) 1.1702(7) 0.7618(6) 0.0220(14) Uani 1 1 d . . . . .
O3 O 1.0110(8) 0.5632(8) 0.3503(7) 0.049(2) Uani 1 1 d . . . . .
O4 O 0.9270(6) 0.5242(6) 0.5539(5) 0.0191(14) Uani 1 1 d . . . . .
O1C O 1.9367(8) 1.1957(8) 0.4087(9) 0.045(2) Uani 1 1 d D . . . .
N3C N 2.1441(12) 1.1959(13) 0.4113(11) 0.060(3) Uani 1 1 d D . . . .
C2C C 2.070(2) 1.254(2) 0.401(2) 0.053(7) Uiso 0.5 1 d D . P A 1
C4C C 2.066(3) 1.051(2) 0.447(3) 0.088(11) Uiso 0.5 1 d D . P A 1
C5C C 2.277(2) 1.247(3) 0.404(4) 0.089(12) Uiso 0.5 1 d D . P A 1
C2C1 C 2.020(3) 1.150(3) 0.422(3) 0.046(6) Uiso 0.5 1 d . . P A 2
C4C1 C 2.264(3) 1.167(4) 0.433(3) 0.066(9) Uiso 0.5 1 d . . P A 2
C5C1 C 2.231(3) 1.368(3) 0.351(3) 0.048(6) Uiso 0.5 1 d . . P A 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
Ba1 O4 2.653(6) 3_774 ?
Ba1 O1C 2.666(7) . ?
Ba1 O1 2.678(6) . ?
Ba1 O3 2.689(7) 1_665 ?
Ba1 O2 2.709(6) 2_864 ?
Ba1 O1 2.834(6) 3_784 ?
Ba1 O2 2.884(6) 3_784 ?
Ba1 O4 2.933(6) 1_665 ?
Ba1 C1 3.176(9) 3_784 ?
Ba1 C8 3.184(9) 1_665 ?
Ba1 Ba1 4.0877(7) 3_784 ?
Ba1 Ba1 4.0877(7) 2_865 ?
C1 O2 1.243(11) . ?
C1 O1 1.268(10) . ?
C1 C2 1.515(12) . ?
C1 Ba1 3.176(9) 2_865 ?
C2 C3 1.365(12) . ?
C2 C7 1.389(13) . ?
C3 C4 1.403(13) . ?
C4 N1 1.352(13) . ?
C4 C5 1.387(12) . ?
C5 C6 1.382(13) . ?
C5 C8 1.503(12) . ?
C6 C7 1.399(14) . ?
C8 O3 1.265(11) . ?
C8 O4 1.271(10) . ?
C8 Ba1 3.184(9) 1_445 ?
O1 Ba1 2.834(6) 2_865 ?
O2 Ba1 2.709(6) 3_785 ?
O2 Ba1 2.884(6) 2_865 ?
O3 Ba1 2.689(7) 1_445 ?
O4 Ba1 2.653(6) 2_755 ?
O4 Ba1 2.933(6) 1_445 ?
O1C C2C1 1.23(3) . ?
O1C C2C 1.26(2) . ?
N3C C2C1 1.18(3) . ?
N3C C2C 1.243(17) . ?
N3C C5C 1.262(18) . ?
N3C C4C 1.409(19) . ?
N3C C4C1 1.49(3) . ?
N3C C5C1 1.73(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
O4 Ba1 O1C 89.7(2) 3_774 . ?
O4 Ba1 O1 90.39(17) 3_774 . ?
O1C Ba1 O1 93.8(2) . . ?
O4 Ba1 O3 146.5(2) 3_774 1_665 ?
O1C Ba1 O3 87.0(3) . 1_665 ?
O1 Ba1 O3 123.1(2) . 1_665 ?
O4 Ba1 O2 68.47(18) 3_774 2_864 ?
O1C Ba1 O2 96.0(2) . 2_864 ?
O1 Ba1 O2 156.58(19) . 2_864 ?
O3 Ba1 O2 78.8(2) 1_665 2_864 ?
O4 Ba1 O1 78.77(18) 3_774 3_784 ?
O1C Ba1 O1 165.5(2) . 3_784 ?
O1 Ba1 O1 95.08(7) . 3_784 ?
O3 Ba1 O1 97.6(2) 1_665 3_784 ?
O2 Ba1 O1 71.69(18) 2_864 3_784 ?
O4 Ba1 O2 116.48(18) 3_774 3_784 ?
O1C Ba1 O2 149.1(2) . 3_784 ?
O1 Ba1 O2 71.34(18) . 3_784 ?
O3 Ba1 O2 79.6(2) 1_665 3_784 ?
O2 Ba1 O2 108.32(16) 2_864 3_784 ?
O1 Ba1 O2 45.31(17) 3_784 3_784 ?
O4 Ba1 O4 166.68(18) 3_774 1_665 ?
O1C Ba1 O4 88.2(2) . 1_665 ?
O1 Ba1 O4 76.64(16) . 1_665 ?
O3 Ba1 O4 46.46(19) 1_665 1_665 ?
O2 Ba1 O4 124.84(17) 2_864 1_665 ?
O1 Ba1 O4 105.03(17) 3_784 1_665 ?
O2 Ba1 O4 62.48(17) 3_784 1_665 ?
O4 Ba1 C1 100.9(2) 3_774 3_784 ?
O1C Ba1 C1 169.3(2) . 3_784 ?
O1 Ba1 C1 87.2(2) . 3_784 ?
O3 Ba1 C1 83.5(3) 1_665 3_784 ?
O2 Ba1 C1 87.1(2) 2_864 3_784 ?
O1 Ba1 C1 23.5(2) 3_784 3_784 ?
O2 Ba1 C1 23.0(2) 3_784 3_784 ?
O4 Ba1 C1 81.70(19) 1_665 3_784 ?
O4 Ba1 C8 169.0(2) 3_774 1_665 ?
O1C Ba1 C8 86.7(3) . 1_665 ?
O1 Ba1 C8 100.2(2) . 1_665 ?
O3 Ba1 C8 22.9(2) 1_665 1_665 ?
O2 Ba1 C8 101.6(2) 2_864 1_665 ?
O1 Ba1 C8 103.0(2) 3_784 1_665 ?
O2 Ba1 C8 70.3(2) 3_784 1_665 ?
O4 Ba1 C8 23.53(19) 1_665 1_665 ?
C1 Ba1 C8 82.7(2) 3_784 1_665 ?
O4 Ba1 Ba1 45.70(12) 3_774 3_784 ?
O1C Ba1 Ba1 124.93(19) . 3_784 ?
O1 Ba1 Ba1 113.02(13) . 3_784 ?
O3 Ba1 Ba1 112.40(18) 1_665 3_784 ?
O2 Ba1 Ba1 44.74(13) 2_864 3_784 ?
O1 Ba1 Ba1 40.68(12) 3_784 3_784 ?
O2 Ba1 Ba1 85.96(13) 3_784 3_784 ?
O4 Ba1 Ba1 142.88(11) 1_665 3_784 ?
C1 Ba1 Ba1 63.87(17) 3_784 3_784 ?
C8 Ba1 Ba1 130.19(17) 1_665 3_784 ?
O4 Ba1 Ba1 129.21(12) 3_774 2_865 ?
O1C Ba1 Ba1 109.7(2) . 2_865 ?
O1 Ba1 Ba1 43.62(12) . 2_865 ?
O3 Ba1 Ba1 82.81(16) 1_665 2_865 ?
O2 Ba1 Ba1 147.44(13) 2_864 2_865 ?
O1 Ba1 Ba1 84.58(12) 3_784 2_865 ?
O2 Ba1 Ba1 41.38(12) 3_784 2_865 ?
O4 Ba1 Ba1 40.36(11) 1_665 2_865 ?
C1 Ba1 Ba1 64.21(17) 3_784 2_865 ?
C8 Ba1 Ba1 61.69(17) 1_665 2_865 ?
Ba1 Ba1 Ba1 123.137(17) 3_784 2_865 ?
O2 C1 O1 122.6(8) . . ?
O2 C1 C2 119.5(8) . . ?
O1 C1 C2 117.9(8) . . ?
O2 C1 Ba1 65.2(5) . 2_865 ?
O1 C1 Ba1 62.9(5) . 2_865 ?
C2 C1 Ba1 156.3(6) . 2_865 ?
C3 C2 C7 119.6(9) . . ?
C3 C2 C1 120.3(8) . . ?
C7 C2 C1 119.9(8) . . ?
C2 C3 C4 122.7(8) . . ?
N1 C4 C5 122.6(9) . . ?
N1 C4 C3 119.1(9) . . ?
C5 C4 C3 118.4(9) . . ?
C6 C5 C4 118.6(9) . . ?
C6 C5 C8 119.9(8) . . ?
C4 C5 C8 121.5(8) . . ?
C5 C6 C7 122.9(9) . . ?
C2 C7 C6 117.8(9) . . ?
O3 C8 O4 123.0(8) . . ?
O3 C8 C5 118.8(8) . . ?
O4 C8 C5 118.2(8) . . ?
O3 C8 Ba1 56.0(5) . 1_445 ?
O4 C8 Ba1 67.1(5) . 1_445 ?
C5 C8 Ba1 174.5(6) . 1_445 ?
C1 O1 Ba1 165.7(6) . . ?
C1 O1 Ba1 93.6(5) . 2_865 ?
Ba1 O1 Ba1 95.70(17) . 2_865 ?
C1 O2 Ba1 169.4(6) . 3_785 ?
C1 O2 Ba1 91.8(5) . 2_865 ?
Ba1 O2 Ba1 93.88(18) 3_785 2_865 ?
C8 O3 Ba1 101.1(5) . 1_445 ?
C8 O4 Ba1 150.1(6) . 2_755 ?
C8 O4 Ba1 89.4(5) . 1_445 ?
Ba1 O4 Ba1 93.94(17) 2_755 1_445 ?
C2C1 O1C Ba1 173.4(14) . . ?
C2C O1C Ba1 128.6(10) . . ?
C2C N3C C5C 131.1(19) . . ?
C2C N3C C4C 113.8(15) . . ?
C5C N3C C4C 114.9(16) . . ?
C2C1 N3C C4C1 145(2) . . ?
C2C1 N3C C5C1 112.3(17) . . ?
C4C1 N3C C5C1 102.5(16) . . ?
N3C C2C O1C 127.7(19) . . ?
N3C C2C1 O1C 137(2) . . ?

_refine_diff_density_max         1.433
_refine_diff_density_min         -0.712
_refine_diff_density_rms         0.144

_shelxl_version_number           2014-3


# start Validation Reply Form
_vrf_PLAT043_Compound3           
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..       7.07 Check 
RESPONSE: The ccordinated DMF molecule is disordered into two 
coplanar disposiitions, so hydrogen atoms have not been included in the model
to avoid inconsistencies.
;
_vrf_PLAT213_Compound3           
;
PROBLEM: Atom N1              has ADP max/min Ratio .....        4.5 prolat
RESPONSE: Some atoms of the ligand are affected by the disorder of disordered
DMF molecules.
;
# end Validation Reply Form

_exptl_crystal_preparation       Luminescent
####################################################################### 
# 
# 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_Compound2
_database_code_depnum_ccdc_archive 'CCDC 1583252'
_audit_update_record             
;
2018-06-10 deposited with the CCDC.
2018-07-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014

_chemical_name_systematic        
"poly-{[diaqua(mu-1,4-benzenedicarboxylate-k2O,O':k2O'',O''')(mu6-1,4-benzenedicarboxylate-?O:?2O,O':?O':?O'':?2O'',O''':?O''' ) bis(dimethylformamide)dicalcium(II)] tetrahydrate}"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C11 H13 Ca N O6, 2 (H2 O)'
_chemical_formula_sum            'C11 H17 Ca N O8'
_chemical_formula_weight         331.33

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'
Ca Ca 0.2262 0.3064 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   12.540(5)
_cell_length_b                   6.683(5)
_cell_length_c                   19.460(5)
_cell_angle_alpha                90
_cell_angle_beta                 116.17(2)
_cell_angle_gamma                90
_cell_volume                     1463.7(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7661
_cell_measurement_theta_min      2.332
_cell_measurement_theta_max      28.760

# SQUEEZE RESULTS (Version = 160617)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 -0.084 0.750 106 23 ' '
2 0.500 -0.041 0.250 107 23 ' '
# Missing Reflections Below sin(th)/lambda = 0.25
loop_
_platon_missing_refln_index_h
_platon_missing_refln_index_k
_platon_missing_refln_index_l
_platon_missing_refln_theta
1 0 0 1.809
-1 0 2 2.234
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
TITL shelx     P 21/c       R = 0.08
CELL   12.5400    6.6830   19.4600     90.00    116.17     90.00
SPGR P21/c
# Solvent Accessible Volume =       212
# Electrons Found in S.A.V. =        45
# Note: Atoms in Void are Labelled as Cxxx and Qxxx for all Others
C101 0.372 0.547 0.300 !       4.78 eA-3
Q102 0.424 0.530 0.238 !       2.51 eA-3
Q103 0.340 0.462 0.643 !       2.02 eA-3
Q104 0.279 1.017 0.172 !       1.98 eA-3
C105 0.485 0.297 0.292 !       1.56 eA-3
Q106 0.454 0.946 0.159 !       1.43 eA-3
Q107 0.326 0.536 0.246 !       1.43 eA-3
Q108 0.515 0.400 0.262 !       1.17 eA-3
C109 0.558 0.265 0.282 !       0.86 eA-3
Q110 0.595 0.895 0.224 !       0.83 eA-3
C111 0.592 0.147 0.219 !       0.82 eA-3
Q112 0.512 0.503 0.215 !       0.72 eA-3
;


_exptl_crystal_description       prismatic
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_density_method    none
_exptl_crystal_F_000             696
_exptl_absorpt_coefficient_mu    0.466
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
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)
;
_exptl_absorpt_correction_T_min  0.920
_exptl_absorpt_correction_T_max  0.960

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Venture'
_diffrn_measurement_method       ω
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            7661
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.332
_diffrn_reflns_theta_max         28.760
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             3752
_reflns_number_gt                3243
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 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.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;Crystal structure of this compound contains disordered crystallization water molecules 
occupying the voids that could not be refined in their original positions. Instead,
SQUEEZE routine was applied to subtract the residual density and the subsequent calculated 
hkl file was employed during the last cycles of the refinement. This is the reason
why chemical formula does not fit the crystallographic formula.,SQUEEZE
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0869P)²+2.1275P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3752
_refine_ls_number_parameters     174
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0502
_refine_ls_wR_factor_ref         0.1543
_refine_ls_wR_factor_gt          0.1472
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_restrained_S_all      1.061
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ca1 Ca 0.05758(3) 0.47144(6) 0.72523(2) 0.00749(14) Uani 1 1 d . . . . .
C1A C -0.01430(17) 0.4740(3) 0.84728(11) 0.0076(4) Uani 1 1 d . . . . .
C2A C -0.00670(18) 0.4872(3) 0.92649(12) 0.0098(4) Uani 1 1 d . . . . .
C3A C -0.0416(2) 0.3256(3) 0.95748(12) 0.0146(4) Uani 1 1 d . . . . .
H3A H -0.0693 0.2089 0.9291 0.018 Uiso 1 1 calc R U . . .
C4A C 0.0351(2) 0.6614(3) 0.96953(12) 0.0141(4) Uani 1 1 d . . . . .
H4A H 0.0587 0.7692 0.9493 0.017 Uiso 1 1 calc R U . . .
C1B C 0.28343(19) 0.4782(3) 0.85812(13) 0.0131(4) Uani 1 1 d . . . . .
C2B C 0.39543(19) 0.4892(3) 0.93175(13) 0.0133(4) Uani 1 1 d . . . . .
C4B C 0.4610(2) 0.3171(3) 0.96425(13) 0.0182(5) Uani 1 1 d . . . . .
H4B H 0.4349 0.1941 0.9404 0.022 Uiso 1 1 calc R U . . .
C3B C 0.4353(2) 0.6721(3) 0.96812(13) 0.0179(5) Uani 1 1 d . . . . .
H3B H 0.3921 0.7879 0.9469 0.022 Uiso 1 1 calc R U . . .
O1A O -0.01192(14) 0.6332(2) 0.81347(8) 0.0118(3) Uani 1 1 d . . . . .
O2A O -0.01841(14) 0.3056(2) 0.81783(8) 0.0123(3) Uani 1 1 d . . . . .
O1B O 0.23588(15) 0.6382(3) 0.82491(10) 0.0214(4) Uani 1 1 d . . . . .
O2B O 0.24048(16) 0.3105(3) 0.83073(10) 0.0245(4) Uani 1 1 d . . . . .
O1C O 0.17624(15) 0.4435(3) 0.65909(10) 0.0192(4) Uani 1 1 d . . . . .
C2C C 0.2348(3) 0.2953(5) 0.65903(18) 0.0339(6) Uani 1 1 d . . . A 1
H2C H 0.2423 0.1937 0.6935 0.041 Uiso 1 1 calc R U . A 1
N3C N 0.2879(3) 0.2682(5) 0.61420(19) 0.0495(8) Uani 1 1 d . . . A 1
C4C C 0.2785(4) 0.4082(8) 0.5579(3) 0.0712(16) Uani 1 1 d . . . A 1
H4C1 H 0.2314 0.3528 0.5080 0.107 Uiso 1 1 calc R U . A 1
H4C2 H 0.3563 0.4397 0.5630 0.107 Uiso 1 1 calc R U . A 1
H4C3 H 0.2413 0.5278 0.5642 0.107 Uiso 1 1 calc R U . A 1
C5C C 0.3500(5) 0.0802(8) 0.6166(3) 0.0790(16) Uani 1 1 d . . . A 1
H5C1 H 0.3402 -0.0108 0.6516 0.118 Uiso 1 1 calc R U . A 1
H5C2 H 0.4330 0.1067 0.6335 0.118 Uiso 1 1 calc R U . A 1
H5C3 H 0.3174 0.0217 0.5665 0.118 Uiso 1 1 calc R U . A 1
O1W O -0.14849(14) 0.4717(2) 0.63434(9) 0.0137(3) Uani 1 1 d . . . B 1
H1W1 H -0.1850 0.3740 0.6388 0.021 Uiso 1 1 d . U . C 1
H2W1 H -0.1848 0.5709 0.6369 0.021 Uiso 1 1 d . U . D 1


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ca1 O2A 2.360(2) 2_556 ?
Ca1 O1C 2.3653(18) . ?
Ca1 O1A 2.372(2) 2_546 ?
Ca1 O1W 2.4032(19) . ?
Ca1 O1B 2.4856(19) . ?
Ca1 O1A 2.4893(16) . ?
Ca1 O2B 2.5454(19) . ?
Ca1 O2A 2.6264(16) . ?
Ca1 C1B 2.872(2) . ?
Ca1 C1A 2.888(2) . ?
Ca1 Ca1 3.925(2) 2_546 ?
Ca1 Ca1 3.925(2) 2_556 ?
C1A O2A 1.254(3) . ?
C1A O1A 1.258(3) . ?
C1A C2A 1.504(3) . ?
C2A C4A 1.394(3) . ?
C2A C3A 1.398(3) . ?
C3A C4A 1.389(3) 3_567 ?
C3A H3A 0.9300 . ?
C4A C3A 1.389(3) 3_567 ?
C4A H4A 0.9300 . ?
C1B O1B 1.256(3) . ?
C1B O2B 1.256(3) . ?
C1B C2B 1.502(3) . ?
C2B C3B 1.391(3) . ?
C2B C4B 1.393(3) . ?
C4B C3B 1.386(3) 3_667 ?
C4B H4B 0.9300 . ?
C3B C4B 1.386(3) 3_667 ?
C3B H3B 0.9300 . ?
O1A Ca1 2.372(2) 2_556 ?
O2A Ca1 2.360(2) 2_546 ?
O1C C2C 1.234(4) . ?
C2C N3C 1.323(4) . ?
C2C H2C 0.9300 . ?
N3C C4C 1.406(5) . ?
N3C C5C 1.468(5) . ?
C4C H4C1 0.9600 . ?
C4C H4C2 0.9600 . ?
C4C H4C3 0.9600 . ?
C5C H5C1 0.9600 . ?
C5C H5C2 0.9600 . ?
C5C H5C3 0.9600 . ?
O1W H1W1 0.8240 . ?
O1W H2W1 0.8180 . ?

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
O2A Ca1 O1C 87.93(6) 2_556 . ?
O2A Ca1 O1A 143.71(6) 2_556 2_546 ?
O1C Ca1 O1A 82.75(6) . 2_546 ?
O2A Ca1 O1W 75.53(5) 2_556 . ?
O1C Ca1 O1W 109.26(7) . . ?
O1A Ca1 O1W 74.70(5) 2_546 . ?
O2A Ca1 O1B 80.08(6) 2_556 . ?
O1C Ca1 O1B 83.96(7) . . ?
O1A Ca1 O1B 133.10(6) 2_546 . ?
O1W Ca1 O1B 151.56(6) . . ?
O2A Ca1 O1A 75.67(6) 2_556 . ?
O1C Ca1 O1A 154.86(6) . . ?
O1A Ca1 O1A 121.60(4) 2_546 . ?
O1W Ca1 O1A 85.27(6) . . ?
O1B Ca1 O1A 74.64(6) . . ?
O2A Ca1 O2B 131.21(6) 2_556 . ?
O1C Ca1 O2B 81.16(7) . . ?
O1A Ca1 O2B 81.89(6) 2_546 . ?
O1W Ca1 O2B 152.61(6) . . ?
O1B Ca1 O2B 51.65(7) . . ?
O1A Ca1 O2B 95.29(7) . . ?
O2A Ca1 O2A 124.15(4) 2_556 . ?
O1C Ca1 O2A 147.75(6) . . ?
O1A Ca1 O2A 72.89(5) 2_546 . ?
O1W Ca1 O2A 84.69(6) . . ?
O1B Ca1 O2A 97.32(6) . . ?
O1A Ca1 O2A 50.71(6) . . ?
O2B Ca1 O2A 74.86(6) . . ?
O2A Ca1 C1B 105.85(6) 2_556 . ?
O1C Ca1 C1B 83.34(7) . . ?
O1A Ca1 C1B 107.76(6) 2_546 . ?
O1W Ca1 C1B 167.40(6) . . ?
O1B Ca1 C1B 25.83(6) . . ?
O1A Ca1 C1B 83.01(6) . . ?
O2B Ca1 C1B 25.91(6) . . ?
O2A Ca1 C1B 84.32(6) . . ?
O2A Ca1 C1A 101.23(5) 2_556 . ?
O1C Ca1 C1A 161.32(6) . . ?
O1A Ca1 C1A 98.49(5) 2_546 . ?
O1W Ca1 C1A 88.91(6) . . ?
O1B Ca1 C1A 81.67(6) . . ?
O1A Ca1 C1A 25.71(5) . . ?
O2B Ca1 C1A 80.57(7) . . ?
O2A Ca1 C1A 25.72(5) . . ?
C1B Ca1 C1A 78.52(7) . . ?
O2A Ca1 Ca1 148.36(5) 2_556 2_546 ?
O1C Ca1 Ca1 117.02(5) . 2_546 ?
O1A Ca1 Ca1 37.17(4) 2_546 2_546 ?
O1W Ca1 Ca1 77.80(4) . 2_546 ?
O1B Ca1 Ca1 119.45(5) . 2_546 ?
O1A Ca1 Ca1 85.51(5) . 2_546 ?
O2B Ca1 Ca1 74.96(5) . 2_546 ?
O2A Ca1 Ca1 35.73(3) . 2_546 ?
C1B Ca1 Ca1 96.65(5) . 2_546 ?
C1A Ca1 Ca1 61.39(4) . 2_546 ?
O2A Ca1 Ca1 40.54(4) 2_556 2_556 ?
O1C Ca1 Ca1 126.06(5) . 2_556 ?
O1A Ca1 Ca1 145.68(5) 2_546 2_556 ?
O1W Ca1 Ca1 77.73(4) . 2_556 ?
O1B Ca1 Ca1 74.25(5) . 2_556 ?
O1A Ca1 Ca1 35.14(3) . 2_556 ?
O2B Ca1 Ca1 117.38(5) . 2_556 ?
O2A Ca1 Ca1 84.64(5) . 2_556 ?
C1B Ca1 Ca1 95.11(5) . 2_556 ?
C1A Ca1 Ca1 60.72(4) . 2_556 ?
Ca1 Ca1 Ca1 116.70(5) 2_546 2_556 ?
O2A C1A O1A 121.71(19) . . ?
O2A C1A C2A 119.48(17) . . ?
O1A C1A C2A 118.75(17) . . ?
O2A C1A Ca1 65.39(11) . . ?
O1A C1A Ca1 59.14(10) . . ?
C2A C1A Ca1 160.25(13) . . ?
C4A C2A C3A 119.48(19) . . ?
C4A C2A C1A 120.09(18) . . ?
C3A C2A C1A 120.43(18) . . ?
C4A C3A C2A 120.29(19) 3_567 . ?
C4A C3A H3A 119.9 3_567 . ?
C2A C3A H3A 119.9 . . ?
C3A C4A C2A 120.23(19) 3_567 . ?
C3A C4A H4A 119.9 3_567 . ?
C2A C4A H4A 119.9 . . ?
O1B C1B O2B 121.6(2) . . ?
O1B C1B C2B 118.8(2) . . ?
O2B C1B C2B 119.6(2) . . ?
O1B C1B Ca1 59.61(12) . . ?
O2B C1B Ca1 62.34(12) . . ?
C2B C1B Ca1 174.57(16) . . ?
C3B C2B C4B 119.2(2) . . ?
C3B C2B C1B 120.2(2) . . ?
C4B C2B C1B 120.6(2) . . ?
C3B C4B C2B 120.5(2) 3_667 . ?
C3B C4B H4B 119.7 3_667 . ?
C2B C4B H4B 119.7 . . ?
C4B C3B C2B 120.3(2) 3_667 . ?
C4B C3B H3B 119.8 3_667 . ?
C2B C3B H3B 119.8 . . ?
C1A O1A Ca1 156.06(14) . 2_556 ?
C1A O1A Ca1 95.15(12) . . ?
Ca1 O1A Ca1 107.69(6) 2_556 . ?
C1A O2A Ca1 166.44(14) . 2_546 ?
C1A O2A Ca1 88.89(12) . . ?
Ca1 O2A Ca1 103.74(6) 2_546 . ?
C1B O1B Ca1 94.56(14) . . ?
C1B O2B Ca1 91.75(14) . . ?
C2C O1C Ca1 125.57(18) . . ?
O1C C2C N3C 125.7(3) . . ?
O1C C2C H2C 117.1 . . ?
N3C C2C H2C 117.1 . . ?
C2C N3C C4C 121.9(3) . . ?
C2C N3C C5C 120.7(3) . . ?
C4C N3C C5C 117.1(3) . . ?
N3C C4C H4C1 109.5 . . ?
N3C C4C H4C2 109.5 . . ?
H4C1 C4C H4C2 109.5 . . ?
N3C C4C H4C3 109.5 . . ?
H4C1 C4C H4C3 109.5 . . ?
H4C2 C4C H4C3 109.5 . . ?
N3C C5C H5C1 109.5 . . ?
N3C C5C H5C2 109.5 . . ?
H5C1 C5C H5C2 109.5 . . ?
N3C C5C H5C3 109.5 . . ?
H5C1 C5C H5C3 109.5 . . ?
H5C2 C5C H5C3 109.5 . . ?
Ca1 O1W H1W1 112.9 . . ?
Ca1 O1W H2W1 113.7 . . ?
H1W1 O1W H2W1 106.6 . . ?

_refine_diff_density_max         1.952
_refine_diff_density_min         -0.805
_refine_diff_density_rms         0.110

_shelxl_version_number           2014-3




# start Validation Reply Form
_vrf_CHEMW03_Compound2           
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: Crystal structure of this compound contains disordered crystallization 
water molecules occupying the voids that could not be refined in their original 
positions. Instead, SQUEEZE routine was applied to subtract the residual density 
and the subsequent calculated hkl file was employed during the last cycles of 
the refinement. This is the reason why chemical formula does not fit the 
crystallographic formula.
;
_vrf_PLAT220_Compound2           
;
PROBLEM: Non-Solvent Resd 1   C   Ueq(max)/Ueq(min) Range       10.0 Ratio 
RESPONSE: The structure contains a crystallographically independent DMF 
molecule that is involved in the disorder affecting to crystallization 
water molecules in the voids. Therefore, some ellipsoids and distances are
unusual.
;
_vrf_PLAT230_Compound2           
;
PROBLEM: Hirshfeld Test Diff for    O1C    --  C2C     ..        8.9 s.u.  
RESPONSE: : The structure contains a crystallographically independent DMF 
molecule that is involved in the disorder affecting to crystallization 
water molecules in the voids. Therefore, some ellipsoids and distances are
unusual.
;
# end Validation Reply Form

_exptl_crystal_preparation       Luminescent
