# Electronic Supplementary Material (ESI) for Materials Horizons.
# 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_SER_B6_1_0m
_database_code_depnum_ccdc_archive 'CCDC 1823991'
_audit_update_record             
;
2018-02-14 deposited with the CCDC.
2018-04-19 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT216_SER_B6_1_0m         
;
PROBLEM: Disordered O5W       (An/Solv) ADP max/min Ratio       29.3 Note
RESPONSE: expected disorder in large pores of the MOF
;
_vrf_PLAT430_SER_B6_1_0m         
;
PROBLEM: Short Inter D...A Contact  O1WA     ..O12W             1.84 Ang.
RESPONSE: short intermolecular contacts between water molecules and guest molecules and are unavoidable due to the expected severe disorder of both solvent and guest molecules. 
;
_vrf_PLAT939_SER_B6_1_0m         
;
PROBLEM: Large Value of Not (SHELXL) Weight Optimized S .    2144.64 Check
RESPONSE: related  to intrinsic imperfections quite normal for crystals that suffered a single-crystal to single-crystal process
;
# Added during the CSD deposition process: Wednesday 14 February 2018 10:46 AM
# end Validation Reply Form


_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H106 Ca Cu6 N6 O66'
_chemical_formula_weight         1956.46

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      hexagonal
_space_group_IT_number           173
_space_group_name_H-M_alt        'P 63'
_space_group_name_Hall           'P 6c'

_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, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'

_cell_length_a                   17.8904(16)
_cell_length_b                   17.8904(16)
_cell_length_c                   12.7999(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     3547.9(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    9508
_cell_measurement_theta_min      2.28
_cell_measurement_theta_max      26.8

_exptl_crystal_description       hexagonal-prisms
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.831
_exptl_crystal_F_000             2028
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_exptl_absorpt_coefficient_mu    1.972
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.650
_exptl_absorpt_correction_T_max  0.730
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            76915
_diffrn_reflns_av_unetI/netI     0.0145
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.314
_diffrn_reflns_theta_max         26.958
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5149
_reflns_number_gt                4687
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.912
_reflns_Friedel_fraction_max     1.000
_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 APEX'
_computing_cell_refinement       'Bruker APEX'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0756P)²+5.1694P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_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   0.07(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5149
_refine_ls_number_parameters     331
_refine_ls_number_restraints     79
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0410
_refine_ls_wR_factor_ref         0.1284
_refine_ls_wR_factor_gt          0.1184
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_restrained_S_all      1.094
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ca1 Ca 0.6667 0.3333 0.5644(3) 0.0085(3) Uani 1 3 d S T P . .
Cu1 Cu 0.86369(5) 0.44178(5) 0.43630(5) 0.0228(3) Uani 1 1 d . . . . .
Cu2 Cu 0.86296(5) 0.44594(5) 0.69397(5) 0.0205(2) Uani 1 1 d . . . . .
N1 N 0.9036(4) 0.4011(5) 0.3222(6) 0.0306(16) Uani 1 1 d . . . . .
N2 N 0.9002(4) 0.4074(4) 0.8124(5) 0.0235(13) Uani 1 1 d . . . . .
O1H O 0.82154(18) 0.46356(19) 0.5634(5) 0.0168(6) Uani 1 1 d . . . . .
O1 O 0.9802(3) 0.5500(3) 0.4195(5) 0.0252(12) Uani 1 1 d . . . . .
O2 O 0.7613(3) 0.3224(3) 0.4276(4) 0.0237(11) Uani 1 1 d . . . . .
O3 O 0.7983(4) 0.5015(4) 0.3339(6) 0.0403(17) Uani 1 1 d . . . . .
O4 O 0.9806(3) 0.5549(3) 0.7076(5) 0.0289(13) Uani 1 1 d . . . . .
O5 O 0.7620(3) 0.3247(3) 0.7007(4) 0.0209(10) Uani 1 1 d . . . . .
O6 O 0.7977(4) 0.5068(4) 0.7938(6) 0.0411(17) Uani 1 1 d . . . . .
C1 C 0.7624(5) 0.2755(5) 0.3550(7) 0.0293(18) Uani 1 1 d . . . . .
C2 C 0.8452(6) 0.3126(6) 0.2843(10) 0.051(3) Uani 1 1 d . . . . .
H2 H 0.8300 0.3131 0.2092 0.061 Uiso 1 1 calc R U . . .
C3 C 1.0221(4) 0.5400(5) 0.3459(6) 0.0202(14) Uani 1 1 d . . . . .
C4 C 0.7659(5) 0.2791(5) 0.7775(7) 0.0309(18) Uani 1 1 d . . . . .
C5 C 0.8429(6) 0.3215(5) 0.8501(8) 0.036(2) Uani 1 1 d . . . . .
H5 H 0.8735 0.2877 0.8497 0.044 Uiso 1 1 calc R U . . .
C6 C 1.0209(5) 0.5451(5) 0.7848(7) 0.0244(16) Uani 1 1 d . . . . .
C1H C 0.8883(7) 0.2536(6) 0.3009(14) 0.089(5) Uani 1 1 d . . . . .
H1H1 H 0.8467 0.1939 0.2786 0.107 Uiso 1 1 calc R U . . .
H1H2 H 0.9396 0.2753 0.2552 0.107 Uiso 1 1 calc R U . . .
C2H C 0.8108(7) 0.3236(7) 0.9660(7) 0.063(3) Uani 1 1 d . . . . .
H2A H 0.7704 0.2635 0.9876 0.075 Uiso 1 1 calc R U . . .
H2B H 0.8614 0.3463 1.0131 0.075 Uiso 1 1 calc R U . . .
O2H O 0.9141(7) 0.2515(6) 0.4072(14) 0.122(5) Uani 1 1 d . . . . .
H2H H 0.9002 0.2006 0.4233 0.183 Uiso 1 1 calc R U . . .
O3H O 0.7722(10) 0.3697(10) 0.9811(12) 0.127(4) Uani 1 1 d . . . . .
H3H H 0.7327 0.3450 1.0255 0.190 Uiso 1 1 calc R U . . .
O2W O 0.1821(7) 0.3763(5) 0.0665(13) 0.107(3) Uani 1 1 d . . . . .
O1W O 0.9427(6) 0.3849(6) 0.5670(13) 0.103(3) Uani 1 1 d . . . . .
O3W O 0.3159(8) 0.3289(11) 0.5573(15) 0.173(7) Uani 1 1 d . U . . .
O4W O 0.1541(14) 0.8532(11) 0.5510(17) 0.197(8) Uani 1 1 d . U . . .
O5W O 1.0822(13) 0.3760(15) 0.4302(17) 0.099(7) Uani 0.5 1 d . U P . .
O6W O 0.0831(14) 0.3812(14) 0.698(2) 0.212(10) Uani 1 1 d . U . . .
O7W O 1.098(2) 0.2558(16) 0.211(3) 0.32(2) Uani 1 1 d . U . . .
O8W O 0.1261(12) 0.4828(16) 0.6209(12) 0.174(7) Uani 1 1 d . U . . .
O5WA O 1.0839(12) 0.3325(12) 0.3764(15) 0.081(5) Uani 0.5 1 d . U P . .
O9W O 1.009(7) 0.122(4) 0.164(5) 0.53(5) Uani 1 1 d . U . . .
O11W O 0.938(3) -0.004(6) 0.424(7) 0.31(4) Uani 0.5 1 d . U P . .
O10W O 0.860(4) 0.018(4) 0.104(10) 0.63(6) Uani 1 1 d . U . . .
O12W O 0.848(6) -0.016(7) 0.296(6) 0.74(8) Uani 1 1 d . U . . .
O13W O 0.738(2) 0.018(3) 0.380(5) 0.46(4) Uani 1 1 d . U . . .
O1WA O 0.898(5) 0.076(3) 0.387(5) 0.28(3) Uani 0.5 1 d . U 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
Ca1 O5 2.498(5) 3_665 ?
Ca1 O5 2.498(5) 2_655 ?
Ca1 O5 2.498(5) . ?
Ca1 O2 2.509(6) . ?
Ca1 O2 2.509(6) 3_665 ?
Ca1 O2 2.509(6) 2_655 ?
Ca1 O1H 2.579(3) . ?
Ca1 O1H 2.579(3) 3_665 ?
Ca1 O1H 2.579(3) 2_655 ?
Ca1 Cu1 3.4695(17) . ?
Ca1 Cu1 3.4695(17) 3_665 ?
Ca1 Cu1 3.4695(17) 2_655 ?
Cu1 O1H 1.913(6) . ?
Cu1 N1 1.921(7) . ?
Cu1 O2 2.004(4) . ?
Cu1 O1 2.026(5) . ?
Cu1 O3 2.340(6) . ?
Cu2 O1H 1.918(6) . ?
Cu2 N2 1.917(7) . ?
Cu2 O5 2.014(4) . ?
Cu2 O4 2.039(5) . ?
Cu2 O6 2.335(6) . ?
N1 C6 1.296(10) 4_764 ?
N1 C2 1.477(11) . ?
N2 C3 1.301(9) 4_765 ?
N2 C5 1.439(10) . ?
O1 C3 1.270(9) . ?
O2 C1 1.260(10) . ?
O3 C1 1.240(10) 2_655 ?
O4 C6 1.286(10) . ?
O5 C4 1.302(10) . ?
O6 C4 1.251(10) 2_655 ?
C1 O3 1.240(10) 3_665 ?
C1 C2 1.571(11) . ?
C2 C1H 1.604(18) . ?
C3 N2 1.301(9) 4_764 ?
C3 C6 1.533(7) 4_764 ?
C4 O6 1.251(10) 3_665 ?
C4 C5 1.514(11) . ?
C5 C2H 1.597(14) . ?
C6 N1 1.296(10) 4_765 ?
C6 C3 1.533(7) 4_765 ?
C1H O2H 1.444(19) . ?
C2H O3H 1.328(17) . ?
O5W O5WA 1.05(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
O5 Ca1 O5 76.6(2) 3_665 2_655 ?
O5 Ca1 O5 76.6(2) 3_665 . ?
O5 Ca1 O5 76.6(2) 2_655 . ?
O5 Ca1 O2 137.31(16) 3_665 . ?
O5 Ca1 O2 138.79(17) 2_655 . ?
O5 Ca1 O2 88.57(11) . . ?
O5 Ca1 O2 88.57(11) 3_665 3_665 ?
O5 Ca1 O2 137.31(16) 2_655 3_665 ?
O5 Ca1 O2 138.80(16) . 3_665 ?
O2 Ca1 O2 76.7(2) . 3_665 ?
O5 Ca1 O2 138.79(16) 3_665 2_655 ?
O5 Ca1 O2 88.57(11) 2_655 2_655 ?
O5 Ca1 O2 137.31(16) . 2_655 ?
O2 Ca1 O2 76.7(2) . 2_655 ?
O2 Ca1 O2 76.7(2) 3_665 2_655 ?
O5 Ca1 O1H 135.8(2) 3_665 . ?
O5 Ca1 O1H 72.10(16) 2_655 . ?
O5 Ca1 O1H 66.49(15) . . ?
O2 Ca1 O1H 66.73(16) . . ?
O2 Ca1 O1H 135.4(2) 3_665 . ?
O2 Ca1 O1H 70.88(16) 2_655 . ?
O5 Ca1 O1H 66.49(15) 3_665 3_665 ?
O5 Ca1 O1H 135.8(2) 2_655 3_665 ?
O5 Ca1 O1H 72.10(16) . 3_665 ?
O2 Ca1 O1H 70.88(16) . 3_665 ?
O2 Ca1 O1H 66.73(16) 3_665 3_665 ?
O2 Ca1 O1H 135.4(2) 2_655 3_665 ?
O1H Ca1 O1H 119.999(4) . 3_665 ?
O5 Ca1 O1H 72.10(16) 3_665 2_655 ?
O5 Ca1 O1H 66.49(15) 2_655 2_655 ?
O5 Ca1 O1H 135.8(2) . 2_655 ?
O2 Ca1 O1H 135.4(2) . 2_655 ?
O2 Ca1 O1H 70.88(16) 3_665 2_655 ?
O2 Ca1 O1H 66.73(16) 2_655 2_655 ?
O1H Ca1 O1H 119.996(3) . 2_655 ?
O1H Ca1 O1H 119.997(4) 3_665 2_655 ?
O5 Ca1 Cu1 155.94(13) 3_665 . ?
O5 Ca1 Cu1 104.28(11) 2_655 . ?
O5 Ca1 Cu1 80.26(11) . . ?
O2 Ca1 Cu1 34.69(10) . . ?
O2 Ca1 Cu1 105.00(16) 3_665 . ?
O2 Ca1 Cu1 64.82(11) 2_655 . ?
O1H Ca1 Cu1 32.87(13) . . ?
O1H Ca1 Cu1 100.29(9) 3_665 . ?
O1H Ca1 Cu1 130.85(12) 2_655 . ?
O5 Ca1 Cu1 80.26(11) 3_665 3_665 ?
O5 Ca1 Cu1 155.94(13) 2_655 3_665 ?
O5 Ca1 Cu1 104.28(11) . 3_665 ?
O2 Ca1 Cu1 64.82(11) . 3_665 ?
O2 Ca1 Cu1 34.69(10) 3_665 3_665 ?
O2 Ca1 Cu1 105.00(16) 2_655 3_665 ?
O1H Ca1 Cu1 130.85(12) . 3_665 ?
O1H Ca1 Cu1 32.88(13) 3_665 3_665 ?
O1H Ca1 Cu1 100.29(9) 2_655 3_665 ?
Cu1 Ca1 Cu1 99.50(6) . 3_665 ?
O5 Ca1 Cu1 104.28(11) 3_665 2_655 ?
O5 Ca1 Cu1 80.26(11) 2_655 2_655 ?
O5 Ca1 Cu1 155.94(13) . 2_655 ?
O2 Ca1 Cu1 105.00(16) . 2_655 ?
O2 Ca1 Cu1 64.82(11) 3_665 2_655 ?
O2 Ca1 Cu1 34.69(10) 2_655 2_655 ?
O1H Ca1 Cu1 100.29(9) . 2_655 ?
O1H Ca1 Cu1 130.85(12) 3_665 2_655 ?
O1H Ca1 Cu1 32.88(13) 2_655 2_655 ?
Cu1 Ca1 Cu1 99.50(6) . 2_655 ?
Cu1 Ca1 Cu1 99.50(6) 3_665 2_655 ?
O1H Cu1 N1 169.2(3) . . ?
O1H Cu1 O2 91.19(18) . . ?
N1 Cu1 O2 82.5(3) . . ?
O1H Cu1 O1 102.57(18) . . ?
N1 Cu1 O1 83.2(3) . . ?
O2 Cu1 O1 165.5(2) . . ?
O1H Cu1 O3 92.6(2) . . ?
N1 Cu1 O3 96.4(3) . . ?
O2 Cu1 O3 93.2(2) . . ?
O1 Cu1 O3 90.9(2) . . ?
O1H Cu1 Ca1 47.04(10) . . ?
N1 Cu1 Ca1 127.8(2) . . ?
O2 Cu1 Ca1 45.45(15) . . ?
O1 Cu1 Ca1 148.97(16) . . ?
O3 Cu1 Ca1 85.40(15) . . ?
O1H Cu2 N2 168.7(2) . . ?
O1H Cu2 O5 90.12(18) . . ?
N2 Cu2 O5 82.2(2) . . ?
O1H Cu2 O4 102.51(19) . . ?
N2 Cu2 O4 84.1(2) . . ?
O5 Cu2 O4 165.3(2) . . ?
O1H Cu2 O6 94.4(2) . . ?
N2 Cu2 O6 94.6(3) . . ?
O5 Cu2 O6 95.1(2) . . ?
O4 Cu2 O6 91.5(2) . . ?
O1H Cu2 Ca1 46.95(10) . . ?
N2 Cu2 Ca1 126.97(19) . . ?
O5 Cu2 Ca1 45.06(15) . . ?
O4 Cu2 Ca1 148.91(17) . . ?
O6 Cu2 Ca1 86.30(16) . . ?
C6 N1 C2 126.2(8) 4_764 . ?
C6 N1 Cu1 116.5(6) 4_764 . ?
C2 N1 Cu1 117.3(6) . . ?
C3 N2 C5 126.5(7) 4_765 . ?
C3 N2 Cu2 116.0(6) 4_765 . ?
C5 N2 Cu2 117.3(5) . . ?
Cu1 O1H Cu2 118.93(15) . . ?
Cu1 O1H Ca1 100.09(18) . . ?
Cu2 O1H Ca1 100.14(19) . . ?
C3 O1 Cu1 110.0(4) . . ?
C1 O2 Cu1 116.1(5) . . ?
C1 O2 Ca1 143.4(5) . . ?
Cu1 O2 Ca1 99.9(2) . . ?
C1 O3 Cu1 120.3(5) 2_655 . ?
C6 O4 Cu2 108.4(4) . . ?
C4 O5 Cu2 114.0(4) . . ?
C4 O5 Ca1 144.9(5) . . ?
Cu2 O5 Ca1 100.14(19) . . ?
C4 O6 Cu2 120.6(6) 2_655 . ?
O3 C1 O2 125.4(7) 3_665 . ?
O3 C1 C2 116.6(7) 3_665 . ?
O2 C1 C2 118.0(7) . . ?
N1 C2 C1 106.0(7) . . ?
N1 C2 C1H 110.3(9) . . ?
C1 C2 C1H 107.9(9) . . ?
O1 C3 N2 129.4(7) . 4_764 ?
O1 C3 C6 118.7(5) . 4_764 ?
N2 C3 C6 111.9(6) 4_764 4_764 ?
O6 C4 O5 123.1(7) 3_665 . ?
O6 C4 C5 118.9(7) 3_665 . ?
O5 C4 C5 118.0(6) . . ?
N2 C5 C4 108.3(7) . . ?
N2 C5 C2H 111.1(8) . . ?
C4 C5 C2H 109.6(8) . . ?
O4 C6 N1 129.0(7) . 4_765 ?
O4 C6 C3 119.4(5) . 4_765 ?
N1 C6 C3 111.6(6) 4_765 4_765 ?
O2H C1H C2 114.0(9) . . ?
O3H C2H C5 117.0(11) . . ?

_refine_diff_density_max         0.961
_refine_diff_density_min         -0.993
_refine_diff_density_rms         0.256

_shelxl_version_number           2013-4


_exptl_crystal_recrystallization_method 'slow diffusion'
####################################################################### 
# 
# 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_ser17b_0m
_database_code_depnum_ccdc_archive 'CCDC 1823995'
_audit_update_record             
;
2018-02-14 deposited with the CCDC.
2018-04-19 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_CHEMW03_ser17b_0m           
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: The solvent molecules were highly disordered not all the ones detected by TGA analysis, have been modeled but anyway all the ones detected have been added in final formula 
;
_vrf_SHFSU01_ser17b_0m           
;
PROBLEM: The absolute value of parameter shift to su ratio > 0.20
RESPONSE: C1L and C7L exhibit parameters constantly oscillating. It is due to disorder of guest molecule
;
_vrf_PLAT043_ser17b_0m           
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..     264.85 Check
RESPONSE: The solvent molecules were highly disordered not all the ones detected by TGA analysis, have been modeled but anyway all the ones detected have been added in final formula 
;
_vrf_PLAT080_ser17b_0m           
;
PROBLEM: Maximum Shift/Error ............................       0.31 Why ?
RESPONSE: C1L and C7L exhibit parameters constantly oscillating. It is due to disorder of guest molecule
;
_vrf_PLAT211_ser17b_0m           
;
PROBLEM: ADP of Atom C1L       is N.P.D. or (nearly) 2D .     Please Check
RESPONSE: Unavoidable for disorder
;
_vrf_PLAT213_ser17b_0m           
;
PROBLEM: Atom C2H             has ADP max/min Ratio .....        7.6 prolat
RESPONSE: Disorder on terminal serine moiety pointing within pores
;
_vrf_PLAT234_ser17b_0m           
;
PROBLEM: Large Hirshfeld Difference O2H      --C2H              0.63 Ang.
RESPONSE: Disorder on terminal serine moiety pointing within pores
;
_vrf_PLAT939_ser17b_0m           
;
PROBLEM: Large Value of Not (SHELXL) Weight Optimized S .    3313.47 Check
RESPONSE: It is related  to intrinsic imperfections quite normal for crystals that suffered a single-crystal to single-crystal process
;
# Added during the CSD deposition process: Wednesday 14 February 2018 10:46 AM
# end Validation Reply Form


_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48.40 H80.20 Ca Cu6 N11 O37.60'
_chemical_formula_weight         1839.15

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      hexagonal
_space_group_IT_number           173
_space_group_name_H-M_alt        'P 63'
_space_group_name_Hall           'P 6c'

_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, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'

_cell_length_a                   17.9504(13)
_cell_length_b                   17.9504(13)
_cell_length_c                   12.5603(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     3504.9(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    9945
_cell_measurement_theta_min      2.27
_cell_measurement_theta_max      27.29

_exptl_crystal_description       hexagonal-prisms
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.743
_exptl_crystal_F_000             1885
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_exptl_absorpt_coefficient_mu    1.964
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.644
_exptl_absorpt_correction_T_max  0.721
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
__diffrn_source                  'fine-focus sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            48081
_diffrn_reflns_av_unetI/netI     0.0281
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.310
_diffrn_reflns_theta_max         27.731
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5438
_reflns_number_gt                4591
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.905
_reflns_Friedel_fraction_max     0.980
_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 APEX'
_computing_cell_refinement       'Bruker APEX'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1464P)²+13.7824P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1971 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.072(15)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5438
_refine_ls_number_parameters     338
_refine_ls_number_restraints     237
_refine_ls_R_factor_all          0.0737
_refine_ls_R_factor_gt           0.0613
_refine_ls_wR_factor_ref         0.2052
_refine_ls_wR_factor_gt          0.1906
_refine_ls_goodness_of_fit_ref   0.953
_refine_ls_restrained_S_all      1.307
_refine_ls_shift/su_max          0.305
_refine_ls_shift/su_mean         0.004

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 0.44171(7) 0.86126(7) 0.51713(12) 0.0219(3) Uani 1 1 d . . . . .
Cu2 Cu 0.13968(7) 0.58678(7) 0.25259(12) 0.0205(3) Uani 1 1 d . . . . .
Ca1 Ca 0.3333 0.6667 0.3860(4) 0.0122(4) Uani 1 3 d S T P . .
O1 O 0.3222(4) 0.7603(4) 0.5249(7) 0.0229(14) Uani 1 1 d . . . . .
O4 O 0.2385(4) 0.5635(4) 0.2462(7) 0.0228(14) Uani 1 1 d . . . . .
O2 O 0.5499(4) 0.9784(4) 0.5303(7) 0.0257(17) Uani 1 1 d . . . . .
O1HH O 0.4638(3) 0.8194(3) 0.3865(8) 0.0193(9) Uani 1 1 d . . . . .
O6 O 0.0227(4) 0.5786(5) 0.2418(8) 0.0288(17) Uani 1 1 d . . . . .
O5 O 0.2012(5) 0.7116(6) 0.1539(9) 0.041(2) Uani 1 1 d . . . . .
N1 N 0.3990(6) 0.9015(5) 0.6331(8) 0.0269(19) Uani 1 1 d . . . . .
N2 N 0.0980(6) 0.5077(7) 0.1354(8) 0.030(2) Uani 1 1 d . . . . .
C4 C 0.2316(7) 0.5130(8) 0.1700(11) 0.032(3) Uani 1 1 d . . . . .
C1 C 0.2742(7) 0.7613(7) 0.5997(10) 0.028(2) Uani 1 1 d . . . . .
C2 C 0.3116(8) 0.8467(9) 0.6682(13) 0.045(3) Uani 1 1 d . . . . .
H2A H 0.3113 0.8327 0.7452 0.054 Uiso 1 1 calc R U . . .
C5 C 0.1561(7) 0.4797(9) 0.0939(10) 0.035(3) Uani 1 1 d D . . . .
H5A H 0.1265 0.4157 0.0867 0.042 Uiso 1 1 calc R U . . .
C6 C -0.0206(6) 0.5251(7) 0.1674(10) 0.024(2) Uani 1 1 d . . . . .
O3 O 0.2017(5) 0.7037(6) 0.6201(8) 0.038(2) Uani 1 1 d . . . . .
C3 C 0.5396(7) 1.0205(7) 0.6041(9) 0.025(2) Uani 1 1 d . . . . .
O1H O 0.2499(12) 0.9130(11) 0.5432(17) 0.120(7) Uani 1 1 d D U . . .
C1H C 0.2527(8) 0.8874(9) 0.6506(17) 0.098(9) Uani 1 1 d D U . . .
C2H C 0.1941(14) 0.529(2) -0.0230(11) 0.206(18) Uani 1 1 d D U . . .
O2H O 0.187(4) 0.523(4) -0.1386(17) 0.55(4) Uani 1 1 d D U . . .
O1W O 0.075(2) 0.460(4) 0.400(4) 0.38(3) Uani 1 1 d . U . . .
O2W O 0.1768(11) 0.8049(9) 0.383(2) 0.119(5) Uani 1 1 d . . . . .
O3W O 0.0032(9) 0.3211(13) -0.1002(18) 0.134(8) Uani 1 1 d . . . . .
C5L C 0.073(2) 0.7395(19) -0.1002(19) 0.079(11) Uani 0.2667 1 d DG U P . .
C6L C 0.089(2) 0.702(2) -0.1876(15) 0.065(10) Uani 0.2667 1 d DG U P . .
C1L C 0.1181(18) 0.6439(16) -0.172(2) 0.041(7) Uani 0.2667 1 d DG U P . .
C2L C 0.131(2) 0.6237(18) -0.070(3) 0.071(11) Uani 0.2667 1 d DG U P . .
C3L C 0.116(2) 0.6613(18) 0.0173(18) 0.074(11) Uani 0.2667 1 d G U P . .
C4L C 0.0867(16) 0.7193(15) 0.0022(16) 0.026(6) Uani 0.2667 1 d DG U P . .
C10L C 0.119(5) 0.838(2) -0.120(2) 0.24(5) Uani 0.2667 1 d D U P . .
C9L C 0.190(3) 0.904(2) -0.051(4) 0.24(5) Uani 0.2667 1 d D U P . .
C7L C 0.101(3) 0.787(2) 0.088(2) 0.23(5) Uani 0.2667 1 d D U P . .
C8L C 0.120(3) 0.875(2) 0.041(3) 0.25(5) Uani 0.2667 1 d D U P . .
C12L C 0.090(3) 0.865(3) 0.277(3) 0.094 Uiso 0.2667 1 d D U P . .
C11L C 0.098(5) 0.798(4) 0.208(2) 0.750 Uiso 0.2667 1 d D U P . .
C14L C 0.068(4) 0.912(4) 0.089(4) 0.162 Uiso 0.2667 1 d D U P . .
C13L C 0.040(3) 0.891(2) 0.200(3) 0.237 Uiso 0.2667 1 d D U P . .
C16L C 0.0000 1.0000 0.136(6) 0.313 Uiso 0.8 3 d DS U P . .
C17L C 0.024(5) 0.960(4) 0.044(5) 0.176 Uiso 0.2667 1 d D U P . .
C15L C 0.039(3) 0.971(3) 0.241(5) 0.227 Uiso 0.2667 1 d D U P . .
C1M C -0.052(3) 0.825(2) 0.215(5) 0.25(9) Uani 0.2667 1 d D U P . .
O1L O 0.133(3) 0.608(3) -0.256(3) 0.424 Uiso 0.2667 1 d D U P . .
O1M O -0.002(7) 0.976(6) 0.333(5) 0.43(9) Uani 0.2667 1 d D U P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O1HH 1.927(8) . ?
Cu1 N1 1.945(10) . ?
Cu1 O1 2.002(6) . ?
Cu1 O2 2.033(7) . ?
Cu1 O3 2.312(9) 3_565 ?
Cu1 Ca1 3.450(2) . ?
Cu2 N2 1.918(9) . ?
Cu2 O1HH 1.917(9) 2_665 ?
Cu2 O4 2.016(6) . ?
Cu2 O6 2.035(7) . ?
Cu2 O5 2.303(9) . ?
Cu2 Ca1 3.459(2) . ?
Ca1 O1 2.498(8) . ?
Ca1 O1 2.498(8) 2_665 ?
Ca1 O1 2.498(8) 3_565 ?
Ca1 O4 2.502(8) 3_565 ?
Ca1 O4 2.502(8) . ?
Ca1 O4 2.502(8) 2_665 ?
Ca1 O1HH 2.565(5) 2_665 ?
Ca1 O1HH 2.565(5) . ?
Ca1 O1HH 2.565(5) 3_565 ?
Ca1 Cu1 3.450(2) 2_665 ?
Ca1 Cu1 3.450(2) 3_565 ?
O1 C1 1.281(14) . ?
O4 C4 1.281(15) . ?
O2 C3 1.267(13) . ?
O1HH Cu2 1.917(9) 3_565 ?
O6 C6 1.285(13) . ?
O5 C4 1.298(13) 3_565 ?
N1 C6 1.319(13) 6_665 ?
N1 C2 1.442(15) . ?
N2 C3 1.286(14) 5_454 ?
N2 C5 1.461(13) . ?
C4 O5 1.298(13) 2_665 ?
C4 C5 1.515(15) . ?
C1 O3 1.217(14) . ?
C1 C2 1.585(15) . ?
C2 C1H 1.57(2) . ?
C5 C2H 1.67(2) . ?
C6 N1 1.319(12) 5_454 ?
C6 C3 1.546(11) 5_454 ?
O3 Cu1 2.312(9) 2_665 ?
C3 N2 1.286(14) 6_665 ?
C3 C6 1.546(11) 6_665 ?
O1H C1H 1.434(13) . ?
C2H O2H 1.458(14) . ?
C5L C6L 1.3900 . ?
C5L C4L 1.3900 . ?
C5L C10L 1.556(14) . ?
C6L C1L 1.3900 . ?
C1L O1L 1.328(9) . ?
C1L C2L 1.3900 . ?
C2L C3L 1.3900 . ?
C3L C4L 1.3900 . ?
C4L C7L 1.551(14) . ?
C10L C9L 1.514(13) . ?
C9L C8L 1.580(14) . ?
C7L C8L 1.558(12) . ?
C7L C11L 1.530(14) . ?
C8L C14L 1.526(12) . ?
C12L C13L 1.540(11) . ?
C12L C11L 1.537(12) . ?
C14L C17L 1.539(13) . ?
C14L C13L 1.466(12) . ?
C13L C15L 1.531(12) . ?
C13L C1M 1.488(14) . ?
C16L C15L 1.681(12) 2_675 ?
C16L C15L 1.681(12) . ?
C16L C15L 1.681(12) 3_465 ?
C16L C17L 1.535(11) 3_465 ?
C16L C17L 1.535(11) 2_675 ?
C16L C17L 1.535(11) . ?
C17L C17L 1.73(6) 3_465 ?
C17L C17L 1.73(6) 2_675 ?
C15L C15L 1.83(6) 2_675 ?
C15L C15L 1.83(6) 3_465 ?
C15L O1M 1.399(14) . ?
C15L O1M 1.58(9) 2_675 ?
O1M O1M 0.71(13) 2_675 ?
O1M O1M 0.71(13) 3_465 ?
O1M C15L 1.58(9) 3_465 ?

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
O1HH Cu1 N1 168.1(4) . . ?
O1HH Cu1 O1 91.4(3) . . ?
N1 Cu1 O1 81.8(3) . . ?
O1HH Cu1 O2 101.3(3) . . ?
N1 Cu1 O2 84.6(3) . . ?
O1 Cu1 O2 165.7(3) . . ?
O1HH Cu1 O3 92.8(3) . 3_565 ?
N1 Cu1 O3 97.5(4) . 3_565 ?
O1 Cu1 O3 94.7(3) . 3_565 ?
O2 Cu1 O3 91.2(3) . 3_565 ?
O1HH Cu1 Ca1 47.19(15) . . ?
N1 Cu1 Ca1 127.3(3) . . ?
O1 Cu1 Ca1 45.6(2) . . ?
O2 Cu1 Ca1 148.1(2) . . ?
O3 Cu1 Ca1 86.4(2) 3_565 . ?
N2 Cu2 O1HH 167.0(4) . 2_665 ?
N2 Cu2 O4 82.7(3) . . ?
O1HH Cu2 O4 90.4(3) 2_665 . ?
N2 Cu2 O6 83.7(4) . . ?
O1HH Cu2 O6 101.6(3) 2_665 . ?
O4 Cu2 O6 164.8(3) . . ?
N2 Cu2 O5 97.3(5) . . ?
O1HH Cu2 O5 94.5(3) 2_665 . ?
O4 Cu2 O5 97.8(3) . . ?
O6 Cu2 O5 90.6(3) . . ?
N2 Cu2 Ca1 128.1(3) . . ?
O1HH Cu2 Ca1 46.92(16) 2_665 . ?
O4 Cu2 Ca1 45.5(2) . . ?
O6 Cu2 Ca1 148.1(2) . . ?
O5 Cu2 Ca1 87.9(2) . . ?
O1 Ca1 O1 76.6(3) . 2_665 ?
O1 Ca1 O1 76.6(3) . 3_565 ?
O1 Ca1 O1 76.6(3) 2_665 3_565 ?
O1 Ca1 O4 88.88(17) . 3_565 ?
O1 Ca1 O4 139.1(2) 2_665 3_565 ?
O1 Ca1 O4 137.2(2) 3_565 3_565 ?
O1 Ca1 O4 137.2(2) . . ?
O1 Ca1 O4 88.88(17) 2_665 . ?
O1 Ca1 O4 139.1(2) 3_565 . ?
O4 Ca1 O4 76.2(3) 3_565 . ?
O1 Ca1 O4 139.1(2) . 2_665 ?
O1 Ca1 O4 137.2(2) 2_665 2_665 ?
O1 Ca1 O4 88.88(17) 3_565 2_665 ?
O4 Ca1 O4 76.2(3) 3_565 2_665 ?
O4 Ca1 O4 76.2(3) . 2_665 ?
O1 Ca1 O1HH 70.4(2) . 2_665 ?
O1 Ca1 O1HH 67.5(2) 2_665 2_665 ?
O1 Ca1 O1HH 135.6(3) 3_565 2_665 ?
O4 Ca1 O1HH 71.6(2) 3_565 2_665 ?
O4 Ca1 O1HH 66.9(2) . 2_665 ?
O4 Ca1 O1HH 135.4(3) 2_665 2_665 ?
O1 Ca1 O1HH 67.5(2) . . ?
O1 Ca1 O1HH 135.6(3) 2_665 . ?
O1 Ca1 O1HH 70.4(2) 3_565 . ?
O4 Ca1 O1HH 66.9(2) 3_565 . ?
O4 Ca1 O1HH 135.4(3) . . ?
O4 Ca1 O1HH 71.6(2) 2_665 . ?
O1HH Ca1 O1HH 120.000(3) 2_665 . ?
O1 Ca1 O1HH 135.6(3) . 3_565 ?
O1 Ca1 O1HH 70.4(2) 2_665 3_565 ?
O1 Ca1 O1HH 67.5(2) 3_565 3_565 ?
O4 Ca1 O1HH 135.4(3) 3_565 3_565 ?
O4 Ca1 O1HH 71.6(2) . 3_565 ?
O4 Ca1 O1HH 66.9(2) 2_665 3_565 ?
O1HH Ca1 O1HH 120.000(5) 2_665 3_565 ?
O1HH Ca1 O1HH 119.999(4) . 3_565 ?
O1 Ca1 Cu1 34.92(15) . . ?
O1 Ca1 Cu1 104.8(2) 2_665 . ?
O1 Ca1 Cu1 64.21(16) 3_565 . ?
O4 Ca1 Cu1 80.87(17) 3_565 . ?
O4 Ca1 Cu1 156.19(18) . . ?
O4 Ca1 Cu1 104.43(15) 2_665 . ?
O1HH Ca1 Cu1 100.05(15) 2_665 . ?
O1HH Ca1 Cu1 33.44(19) . . ?
O1HH Ca1 Cu1 131.06(18) 3_565 . ?
O1 Ca1 Cu1 64.21(16) . 2_665 ?
O1 Ca1 Cu1 34.92(15) 2_665 2_665 ?
O1 Ca1 Cu1 104.8(2) 3_565 2_665 ?
O4 Ca1 Cu1 104.43(15) 3_565 2_665 ?
O4 Ca1 Cu1 80.87(17) . 2_665 ?
O4 Ca1 Cu1 156.19(18) 2_665 2_665 ?
O1HH Ca1 Cu1 33.44(19) 2_665 2_665 ?
O1HH Ca1 Cu1 131.06(18) . 2_665 ?
O1HH Ca1 Cu1 100.05(15) 3_565 2_665 ?
Cu1 Ca1 Cu1 99.10(9) . 2_665 ?
O1 Ca1 Cu1 104.8(2) . 3_565 ?
O1 Ca1 Cu1 64.21(16) 2_665 3_565 ?
O1 Ca1 Cu1 34.92(15) 3_565 3_565 ?
O4 Ca1 Cu1 156.19(18) 3_565 3_565 ?
O4 Ca1 Cu1 104.43(15) . 3_565 ?
O4 Ca1 Cu1 80.87(17) 2_665 3_565 ?
O1HH Ca1 Cu1 131.06(18) 2_665 3_565 ?
O1HH Ca1 Cu1 100.05(15) . 3_565 ?
O1HH Ca1 Cu1 33.44(19) 3_565 3_565 ?
Cu1 Ca1 Cu1 99.10(9) . 3_565 ?
Cu1 Ca1 Cu1 99.10(9) 2_665 3_565 ?
C1 O1 Cu1 116.5(6) . . ?
C1 O1 Ca1 143.3(6) . . ?
Cu1 O1 Ca1 99.5(3) . . ?
C4 O4 Cu2 113.1(6) . . ?
C4 O4 Ca1 146.8(6) . . ?
Cu2 O4 Ca1 99.4(3) . . ?
C3 O2 Cu1 109.1(6) . . ?
Cu1 O1HH Cu2 119.7(2) . 3_565 ?
Cu1 O1HH Ca1 99.4(3) . . ?
Cu2 O1HH Ca1 100.0(3) 3_565 . ?
C6 O6 Cu2 108.6(6) . . ?
C4 O5 Cu2 119.0(8) 3_565 . ?
C6 N1 C2 127.5(11) 6_665 . ?
C6 N1 Cu1 114.3(8) 6_665 . ?
C2 N1 Cu1 118.2(8) . . ?
C3 N2 C5 126.0(10) 5_454 . ?
C3 N2 Cu2 117.3(8) 5_454 . ?
C5 N2 Cu2 116.6(7) . . ?
O4 C4 O5 122.1(10) . 2_665 ?
O4 C4 C5 120.1(9) . . ?
O5 C4 C5 117.8(10) 2_665 . ?
O3 C1 O1 125.7(10) . . ?
O3 C1 C2 117.6(10) . . ?
O1 C1 C2 116.7(9) . . ?
N1 C2 C1H 113.3(12) . . ?
N1 C2 C1 106.5(10) . . ?
C1H C2 C1 108.4(11) . . ?
N2 C5 C4 106.8(9) . . ?
N2 C5 C2H 107.9(11) . . ?
C4 C5 C2H 107.3(10) . . ?
O6 C6 N1 128.2(11) . 5_454 ?
O6 C6 C3 119.5(7) . 5_454 ?
N1 C6 C3 112.2(8) 5_454 5_454 ?
C1 O3 Cu1 119.9(7) . 2_665 ?
O2 C3 N2 129.3(11) . 6_665 ?
O2 C3 C6 119.8(7) . 6_665 ?
N2 C3 C6 110.8(8) 6_665 6_665 ?
O1H C1H C2 114.9(12) . . ?
O2H C2H C5 147(4) . . ?
C6L C5L C4L 120.0 . . ?
C6L C5L C10L 108(2) . . ?
C4L C5L C10L 112.8(16) . . ?
C1L C6L C5L 120.0 . . ?
O1L C1L C2L 120.0(9) . . ?
O1L C1L C6L 120.0(9) . . ?
C2L C1L C6L 120.0 . . ?
C1L C2L C3L 120.0 . . ?
C4L C3L C2L 120.0 . . ?
C3L C4L C5L 120.0 . . ?
C3L C4L C7L 121.1(19) . . ?
C5L C4L C7L 114.9(16) . . ?
C9L C10L C5L 123(2) . . ?
C10L C9L C8L 86.7(12) . . ?
C8L C7L C11L 104.5(16) . . ?
C8L C7L C4L 113.4(15) . . ?
C11L C7L C4L 142(2) . . ?
C9L C8L C14L 135(2) . . ?
C9L C8L C7L 110.2(17) . . ?
C14L C8L C7L 115(2) . . ?
C13L C12L C11L 100.7(11) . . ?
C7L C11L C12L 132.7(15) . . ?
C8L C14L C17L 134(2) . . ?
C8L C14L C13L 118.2(13) . . ?
C17L C14L C13L 107.1(12) . . ?
C12L C13L C15L 111(3) . . ?
C12L C13L C14L 120.0(14) . . ?
C15L C13L C14L 103.8(15) . . ?
C12L C13L C1M 104.8(13) . . ?
C15L C13L C1M 100.4(11) . . ?
C14L C13L C1M 115.1(16) . . ?
C15L C16L C15L 66(2) 2_675 . ?
C15L C16L C15L 66(2) 2_675 3_465 ?
C15L C16L C15L 66(2) . 3_465 ?
C15L C16L C17L 135(3) 2_675 3_465 ?
C15L C16L C17L 150(3) . 3_465 ?
C15L C16L C17L 101.1(12) 3_465 3_465 ?
C15L C16L C17L 101.1(12) 2_675 2_675 ?
C15L C16L C17L 135(3) . 2_675 ?
C15L C16L C17L 150(3) 3_465 2_675 ?
C17L C16L C17L 69(3) 3_465 2_675 ?
C15L C16L C17L 150(3) 2_675 . ?
C15L C16L C17L 101.1(12) . . ?
C15L C16L C17L 135(3) 3_465 . ?
C17L C16L C17L 69(3) 3_465 . ?
C17L C16L C17L 69(3) 2_675 . ?
C17L C17L C17L 59.999(10) 3_465 2_675 ?
C17L C17L C14L 149(4) 3_465 . ?
C17L C17L C14L 138(5) 2_675 . ?
C17L C17L C16L 55.7(13) 3_465 . ?
C17L C17L C16L 55.7(13) 2_675 . ?
C14L C17L C16L 108.6(12) . . ?
C15L C15L C15L 60.00(3) 2_675 3_465 ?
C15L C15L O1M 69(3) 2_675 . ?
C15L C15L O1M 57(3) 3_465 . ?
C15L C15L C16L 57.1(12) 2_675 . ?
C15L C15L C16L 57.1(12) 3_465 . ?
O1M C15L C16L 109(2) . . ?
C15L C15L C13L 160.2(17) 2_675 . ?
C15L C15L C13L 114(4) 3_465 . ?
O1M C15L C13L 126.1(17) . . ?
C16L C15L C13L 103.4(12) . . ?
C15L C15L O1M 48(2) 2_675 2_675 ?
C15L C15L O1M 65(3) 3_465 2_675 ?
O1M C15L O1M 27(5) . 2_675 ?
C16L C15L O1M 100(4) . 2_675 ?
C13L C15L O1M 151(3) . 2_675 ?
C15L O1M O1M 91(10) . 2_675 ?
C15L O1M O1M 119(4) . 3_465 ?
O1M O1M O1M 60.00(2) 2_675 3_465 ?
C15L O1M C15L 75(2) . 3_465 ?
O1M O1M C15L 101(6) 2_675 3_465 ?
O1M O1M C15L 62(7) 3_465 3_465 ?

_refine_diff_density_max         1.669
_refine_diff_density_min         -1.294
_refine_diff_density_rms         0.373

_shelxl_version_number           2013-4


_exptl_crystal_recrystallization_method 'slow diffusion'
####################################################################### 
# 
# 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_SER_C_0m
_database_code_depnum_ccdc_archive 'CCDC 1823992'
_audit_update_record             
;
2018-02-14 deposited with the CCDC.
2018-04-19 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT411_SER_C_0m            
;
PROBLEM: Short Inter H...H Contact  H2HA     ..H6CB             1.64 Ang.
RESPONSE: short intermolecular contacts between guest molecules and the whole network are unavoidable due to the expected severe disorder of both solvent and guest molecules. 
;
_vrf_PLAT417_SER_C_0m            
;
PROBLEM: Short Inter D-H..H-D       H2HC     ..H2HC             1.50 Ang.
RESPONSE: short intermolecular contacts between highly disordered guest molecules 
;
_vrf_PLAT939_SER_C_0m            
;
PROBLEM: Large Value of Not (SHELXL) Weight Optimized S .     954.18 Check
RESPONSE: related either to intrinsic imperfections quite normal for crystals that suffered a single-crystal to single-crystal process
;
# Added during the CSD deposition process: Wednesday 14 February 2018 10:46 AM
# end Validation Reply Form


_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H83 Ca Cu6 N9 O54'
_chemical_formula_weight         1999.49

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      hexagonal
_space_group_IT_number           173
_space_group_name_H-M_alt        'P 63'
_space_group_name_Hall           'P 6c'

_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, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'

_cell_length_a                   17.9607(11)
_cell_length_b                   17.9607(11)
_cell_length_c                   12.6765(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     3541.4(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    9913
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      27.05

_exptl_crystal_description       hexagonal-prisms
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.875
_exptl_crystal_F_000             2048
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_exptl_absorpt_coefficient_mu    1.967
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.621
_exptl_absorpt_correction_T_max  0.765
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            46482
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.309
_diffrn_reflns_theta_max         27.283
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5314
_reflns_number_gt                4514
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.912
_reflns_Friedel_fraction_max     0.998
_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 APEX'
_computing_cell_refinement       'Bruker APEX'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1222P)²+5.7840P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1946 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.060(13)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5314
_refine_ls_number_parameters     355
_refine_ls_number_restraints     239
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0462
_refine_ls_wR_factor_ref         0.1531
_refine_ls_wR_factor_gt          0.1379
_refine_ls_goodness_of_fit_ref   0.891
_refine_ls_restrained_S_all      0.909
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.002

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 0.3333 0.6667 0.9538(3) 0.0117(3) Uani 1 3 d S T P . .
Cu1 Cu 0.44760(5) 0.86155(5) 0.82146(10) 0.0207(3) Uani 1 1 d . . . . .
Cu2 Cu 0.44158(5) 0.86228(5) 1.08373(11) 0.0217(3) Uani 1 1 d . . . . .
O1H O 0.4638(2) 0.8203(2) 0.9544(5) 0.0173(7) Uani 1 1 d . . . . .
N1 N 0.4108(4) 0.9020(4) 0.7033(6) 0.0246(14) Uani 1 1 d . . . . .
N2 N 0.3994(5) 0.9019(4) 1.1977(6) 0.0276(15) Uani 1 1 d . . . . .
O1 O 0.5558(3) 0.9791(3) 0.8100(5) 0.0284(13) Uani 1 1 d . . . . .
O2 O 0.5093(5) 0.7978(4) 0.7241(6) 0.0426(18) Uani 1 1 d . . . . .
O3 O 0.3256(3) 0.7619(3) 0.8148(5) 0.0224(11) Uani 1 1 d . . . . .
O4 O 0.5006(4) 0.7977(4) 1.1871(6) 0.0376(16) Uani 1 1 d . . . . .
O5 O 0.5493(3) 0.9794(3) 1.0976(5) 0.0255(12) Uani 1 1 d . . . . .
O6 O 0.3226(3) 0.7607(3) 1.0901(5) 0.0235(11) Uani 1 1 d . . . . .
C1 C 0.4865(6) 0.7191(5) 0.7388(8) 0.032(2) Uani 1 1 d . . . . .
C2 C 0.3226(5) 0.8450(6) 0.6657(8) 0.034(2) Uani 1 1 d . . . . .
H2A H 0.2894 0.8760 0.6675 0.040 Uiso 1 1 calc R U . . .
C3 C 0.5390(5) 1.0224(5) 1.1704(7) 0.0217(15) Uani 1 1 d . . . . .
C4 C 0.4535(5) 0.9800(5) 1.2328(7) 0.0246(16) Uani 1 1 d . . . . .
C5 C 0.2748(5) 0.7613(5) 1.1653(7) 0.0275(18) Uani 1 1 d . . . . .
C6 C 0.3125(7) 0.8431(6) 1.2373(10) 0.051(3) Uani 1 1 d . . . . .
H6A H 0.3152 0.8272 1.3122 0.061 Uiso 1 1 calc R U . . .
C1H C 0.3219(8) 0.8112(8) 0.5495(9) 0.078(4) Uani 1 1 d D U . . .
H1HA H 0.2615 0.7705 0.5299 0.093 Uiso 1 1 calc R U . . .
H1HB H 0.3434 0.8608 0.5007 0.093 Uiso 1 1 calc R U . . .
O2H O 0.3704(13) 0.7702(13) 0.5327(16) 0.172(7) Uani 1 1 d D U . . .
H2HC H 0.3373 0.7167 0.5310 0.257 Uiso 1 1 calc R U . . .
C2H C 0.2533(8) 0.8838(8) 1.2282(16) 0.103(6) Uani 1 1 d D U . . .
H2HA H 0.1957 0.8424 1.2563 0.123 Uiso 1 1 calc R U . . .
H2HB H 0.2774 0.9360 1.2727 0.123 Uiso 1 1 calc R U . . .
O3H O 0.2440(11) 0.9065(12) 1.1213(17) 0.170(7) Uani 1 1 d D U . . .
H3HA H 0.2682 0.9602 1.1159 0.255 Uiso 1 1 calc R U . . .
O1W O 0.3278(9) 0.9893(8) 1.4600(14) 0.062(4) Uani 0.5 1 d . . P . .
O2W O 0.3603(12) 1.4776(18) 0.4015(15) 0.230(11) Uani 1 1 d . U . . .
O3W O 0.3723(8) 1.1783(13) 1.452(2) 0.171(6) Uani 1 1 d . U . . .
O4W O 0.4375(12) 1.3811(12) 0.4457(18) 0.174(7) Uani 1 1 d . U . . .
O5W O 0.2863(17) 1.3719(17) 0.579(2) 0.096(7) Uani 0.5 1 d . U P . .
O5WA O 0.247(2) 1.327(2) 0.644(2) 0.130(11) Uani 0.5 1 d . U P . .
C1C C 0.164(3) 1.071(3) 1.544(6) 0.76(5) Uani 0.6667 1 d D U P . .
C2C C 0.136(4) 1.136(4) 1.513(5) 0.73(5) Uani 0.6667 1 d D U P . .
H2CB H 0.0761 1.0915 1.4940 0.880 Uiso 0.6667 1 calc R U P . .
C3C C 0.122(3) 1.113(4) 1.695(5) 0.75(5) Uani 0.6667 1 d D U P . .
C4C C 0.155(3) 1.057(3) 1.655(6) 0.77(5) Uani 0.6667 1 d D U P . .
C5C C 0.155(4) 1.180(4) 1.405(4) 0.69(4) Uani 0.6667 1 d D U P . .
H5CA H 0.1049 1.1455 1.3580 0.824 Uiso 0.6667 1 calc R U P . .
C6C C 0.167(6) 1.269(4) 1.413(7) 0.68(4) Uani 0.6667 1 d D U P . .
H6CA H 0.2287 1.3116 1.4237 0.820 Uiso 0.6667 1 calc R U P . .
H6CB H 0.1484 1.2837 1.3463 0.820 Uiso 0.6667 1 calc R U P . .
O3' O 0.108(5) 1.115(5) 1.792(5) 0.62(5) Uani 0.6667 1 d D U P . .
O1C O 0.190(5) 1.041(4) 1.463(7) 0.76(7) Uani 0.6667 1 d D U P . .
H1CA H 0.2165 1.0801 1.4190 1.137 Uiso 0.6667 1 calc R U P . .
O2C O 0.118(3) 1.274(2) 1.498(4) 0.35(3) Uani 0.6667 1 d D U P . .
H2CA H 0.1120 1.2375 1.5442 0.529 Uiso 0.6667 1 calc R U P . .
O3C O 0.113(4) 1.155(4) 1.613(5) 0.75(5) Uani 0.6667 1 d D U P . .
O4C O 0.173(6) 1.006(6) 1.712(8) 0.82(7) Uani 0.6667 1 d D U P . .
H4CA H 0.1328 0.9549 1.7053 1.229 Uiso 0.6667 1 calc R U P . .
O5C O 0.230(6) 1.189(6) 1.357(6) 0.69(7) Uani 0.6667 1 d D U P . .
H5CB H 0.2216 1.1811 1.2920 1.037 Uiso 0.6667 1 calc R U 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
Ca1 O6 2.491(6) . ?
Ca1 O6 2.491(6) 2_665 ?
Ca1 O6 2.491(6) 3_565 ?
Ca1 O3 2.507(6) . ?
Ca1 O3 2.507(6) 2_665 ?
Ca1 O3 2.507(6) 3_565 ?
Ca1 O1H 2.577(3) 2_665 ?
Ca1 O1H 2.577(3) . ?
Ca1 O1H 2.577(3) 3_565 ?
Ca1 Cu2 3.4650(18) 2_665 ?
Ca1 Cu2 3.4650(18) . ?
Ca1 Cu2 3.4650(18) 3_565 ?
Cu1 O1H 1.921(6) . ?
Cu1 N1 1.921(7) . ?
Cu1 O3 2.022(5) . ?
Cu1 O1 2.038(5) . ?
Cu1 O2 2.309(7) . ?
Cu2 N2 1.926(7) . ?
Cu2 O1H 1.927(6) . ?
Cu2 O6 2.000(5) . ?
Cu2 O5 2.032(5) . ?
Cu2 O4 2.327(7) . ?
N1 C3 1.268(10) 4_674 ?
N1 C2 1.470(10) . ?
N2 C4 1.321(10) . ?
N2 C6 1.467(12) . ?
O1 C4 1.284(10) 4_674 ?
O2 C1 1.274(10) . ?
O3 C1 1.290(11) 2_665 ?
O4 C5 1.228(10) 3_565 ?
O5 C3 1.274(10) . ?
O6 C5 1.286(10) . ?
C1 O3 1.290(11) 3_565 ?
C1 C2 1.521(12) 3_565 ?
C2 C1 1.521(12) 2_665 ?
C2 C1H 1.591(15) . ?
C3 N1 1.268(10) 4_675 ?
C3 C4 1.547(8) . ?
C4 O1 1.284(10) 4_675 ?
C5 O4 1.228(10) 2_665 ?
C5 C6 1.567(11) . ?
C6 C2H 1.565(19) . ?
C1H O2H 1.410(12) . ?
C2H O3H 1.449(13) . ?
O5W O5WA 1.12(4) . ?
C1C O1C 1.352(14) . ?
C1C C4C 1.423(13) . ?
C1C C2C 1.542(14) . ?
C2C O3C 1.424(14) . ?
C2C C5C 1.524(15) . ?
C3C O3' 1.251(14) . ?
C3C O3C 1.351(13) . ?
C3C C4C 1.480(13) . ?
C4C O4C 1.328(13) . ?
C5C O5C 1.411(15) . ?
C5C C6C 1.501(15) . ?
C6C O2C 1.417(14) . ?

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
O6 Ca1 O6 77.2(2) . 2_665 ?
O6 Ca1 O6 77.2(2) . 3_565 ?
O6 Ca1 O6 77.2(2) 2_665 3_565 ?
O6 Ca1 O3 88.59(13) . . ?
O6 Ca1 O3 139.03(17) 2_665 . ?
O6 Ca1 O3 137.08(17) 3_565 . ?
O6 Ca1 O3 137.08(17) . 2_665 ?
O6 Ca1 O3 88.59(13) 2_665 2_665 ?
O6 Ca1 O3 139.03(17) 3_565 2_665 ?
O3 Ca1 O3 76.1(2) . 2_665 ?
O6 Ca1 O3 139.03(17) . 3_565 ?
O6 Ca1 O3 137.08(17) 2_665 3_565 ?
O6 Ca1 O3 88.59(13) 3_565 3_565 ?
O3 Ca1 O3 76.1(2) . 3_565 ?
O3 Ca1 O3 76.1(2) 2_665 3_565 ?
O6 Ca1 O1H 70.59(17) . 2_665 ?
O6 Ca1 O1H 66.96(17) 2_665 2_665 ?
O6 Ca1 O1H 135.8(2) 3_565 2_665 ?
O3 Ca1 O1H 72.08(17) . 2_665 ?
O3 Ca1 O1H 66.58(17) 2_665 2_665 ?
O3 Ca1 O1H 135.4(2) 3_565 2_665 ?
O6 Ca1 O1H 66.96(17) . . ?
O6 Ca1 O1H 135.8(2) 2_665 . ?
O6 Ca1 O1H 70.59(17) 3_565 . ?
O3 Ca1 O1H 66.57(17) . . ?
O3 Ca1 O1H 135.4(2) 2_665 . ?
O3 Ca1 O1H 72.08(18) 3_565 . ?
O1H Ca1 O1H 119.998(4) 2_665 . ?
O6 Ca1 O1H 135.8(2) . 3_565 ?
O6 Ca1 O1H 70.59(17) 2_665 3_565 ?
O6 Ca1 O1H 66.96(17) 3_565 3_565 ?
O3 Ca1 O1H 135.4(2) . 3_565 ?
O3 Ca1 O1H 72.08(17) 2_665 3_565 ?
O3 Ca1 O1H 66.58(17) 3_565 3_565 ?
O1H Ca1 O1H 119.999(5) 2_665 3_565 ?
O1H Ca1 O1H 120.000(4) . 3_565 ?
O6 Ca1 Cu2 64.70(12) . 2_665 ?
O6 Ca1 Cu2 34.59(11) 2_665 2_665 ?
O6 Ca1 Cu2 105.13(16) 3_565 2_665 ?
O3 Ca1 Cu2 104.69(12) . 2_665 ?
O3 Ca1 Cu2 80.60(12) 2_665 2_665 ?
O3 Ca1 Cu2 155.77(13) 3_565 2_665 ?
O1H Ca1 Cu2 33.26(14) 2_665 2_665 ?
O1H Ca1 Cu2 131.05(13) . 2_665 ?
O1H Ca1 Cu2 100.07(10) 3_565 2_665 ?
O6 Ca1 Cu2 34.59(11) . . ?
O6 Ca1 Cu2 105.13(16) 2_665 . ?
O6 Ca1 Cu2 64.70(11) 3_565 . ?
O3 Ca1 Cu2 80.59(12) . . ?
O3 Ca1 Cu2 155.77(13) 2_665 . ?
O3 Ca1 Cu2 104.69(12) 3_565 . ?
O1H Ca1 Cu2 100.07(10) 2_665 . ?
O1H Ca1 Cu2 33.26(14) . . ?
O1H Ca1 Cu2 131.05(13) 3_565 . ?
Cu2 Ca1 Cu2 99.27(7) 2_665 . ?
O6 Ca1 Cu2 105.13(16) . 3_565 ?
O6 Ca1 Cu2 64.70(11) 2_665 3_565 ?
O6 Ca1 Cu2 34.59(11) 3_565 3_565 ?
O3 Ca1 Cu2 155.77(13) . 3_565 ?
O3 Ca1 Cu2 104.69(12) 2_665 3_565 ?
O3 Ca1 Cu2 80.60(12) 3_565 3_565 ?
O1H Ca1 Cu2 131.05(13) 2_665 3_565 ?
O1H Ca1 Cu2 100.07(10) . 3_565 ?
O1H Ca1 Cu2 33.26(14) 3_565 3_565 ?
Cu2 Ca1 Cu2 99.27(7) 2_665 3_565 ?
Cu2 Ca1 Cu2 99.27(7) . 3_565 ?
O1H Cu1 N1 167.8(3) . . ?
O1H Cu1 O3 90.06(19) . . ?
N1 Cu1 O3 82.9(3) . . ?
O1H Cu1 O1 102.2(2) . . ?
N1 Cu1 O1 83.3(3) . . ?
O3 Cu1 O1 164.6(2) . . ?
O1H Cu1 O2 94.3(2) . . ?
N1 Cu1 O2 96.4(3) . . ?
O3 Cu1 O2 96.6(2) . . ?
O1 Cu1 O2 91.7(2) . . ?
O1H Cu1 Ca1 46.81(11) . . ?
N1 Cu1 Ca1 128.0(2) . . ?
O3 Cu1 Ca1 45.26(15) . . ?
O1 Cu1 Ca1 148.67(17) . . ?
O2 Cu1 Ca1 86.96(16) . . ?
N2 Cu2 O1H 168.3(3) . . ?
N2 Cu2 O6 82.4(3) . . ?
O1H Cu2 O6 90.8(2) . . ?
N2 Cu2 O5 84.2(3) . . ?
O1H Cu2 O5 101.7(2) . . ?
O6 Cu2 O5 166.0(2) . . ?
N2 Cu2 O4 97.1(3) . . ?
O1H Cu2 O4 92.8(2) . . ?
O6 Cu2 O4 93.9(2) . . ?
O5 Cu2 O4 91.8(2) . . ?
N2 Cu2 Ca1 127.3(2) . . ?
O1H Cu2 Ca1 47.17(11) . . ?
O6 Cu2 Ca1 44.98(16) . . ?
O5 Cu2 Ca1 148.43(17) . . ?
O4 Cu2 Ca1 85.80(15) . . ?
Cu1 O1H Cu2 119.63(18) . . ?
Cu1 O1H Ca1 100.3(2) . . ?
Cu2 O1H Ca1 99.6(2) . . ?
C3 N1 C2 125.6(7) 4_674 . ?
C3 N1 Cu1 117.8(6) 4_674 . ?
C2 N1 Cu1 116.3(5) . . ?
C4 N2 C6 127.0(8) . . ?
C4 N2 Cu2 115.3(6) . . ?
C6 N2 Cu2 117.6(6) . . ?
C4 O1 Cu1 108.5(5) 4_674 . ?
C1 O2 Cu1 120.3(6) . . ?
C1 O3 Cu1 113.8(5) 2_665 . ?
C1 O3 Ca1 145.8(5) 2_665 . ?
Cu1 O3 Ca1 99.8(2) . . ?
C5 O4 Cu2 119.9(5) 3_565 . ?
C3 O5 Cu2 109.8(5) . . ?
C5 O6 Cu2 115.8(5) . . ?
C5 O6 Ca1 142.9(5) . . ?
Cu2 O6 Ca1 100.4(2) . . ?
O2 C1 O3 122.5(8) . 3_565 ?
O2 C1 C2 118.5(8) . 3_565 ?
O3 C1 C2 119.0(7) 3_565 3_565 ?
N1 C2 C1 107.8(6) . 2_665 ?
N1 C2 C1H 111.4(8) . . ?
C1 C2 C1H 108.0(8) 2_665 . ?
O5 C3 N1 130.2(8) . 4_675 ?
O5 C3 C4 118.7(5) . . ?
N1 C3 C4 111.0(6) 4_675 . ?
O1 C4 N2 128.8(8) 4_675 . ?
O1 C4 C3 119.3(6) 4_675 . ?
N2 C4 C3 111.9(6) . . ?
O4 C5 O6 126.0(7) 2_665 . ?
O4 C5 C6 116.5(7) 2_665 . ?
O6 C5 C6 117.5(7) . . ?
N2 C6 C2H 111.4(9) . . ?
N2 C6 C5 106.3(7) . . ?
C2H C6 C5 108.6(9) . . ?
O2H C1H C2 116.7(12) . . ?
O3H C2H C6 113.6(11) . . ?
O1C C1C C4C 135.5(16) . . ?
O1C C1C C2C 114.7(18) . . ?
C4C C1C C2C 109.8(14) . . ?
O3C C2C C5C 133(2) . . ?
O3C C2C C1C 101.0(16) . . ?
C5C C2C C1C 123.8(15) . . ?
O3' C3C O3C 131(2) . . ?
O3' C3C C4C 120(2) . . ?
O3C C3C C4C 108.3(11) . . ?
O4C C4C C1C 127.5(17) . . ?
O4C C4C C3C 126.8(19) . . ?
C1C C4C C3C 105.7(10) . . ?
O5C C5C C6C 107.0(14) . . ?
O5C C5C C2C 113.0(16) . . ?
C6C C5C C2C 112(2) . . ?
O2C C6C C5C 110.1(15) . . ?
C3C O3C C2C 115.3(16) . . ?

_refine_diff_density_max         1.318
_refine_diff_density_min         -1.013
_refine_diff_density_rms         0.238

_shelxl_version_number           2013-4


_exptl_crystal_recrystallization_method 'slow diffusion'
####################################################################### 
# 
# 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_SER_B6_0m
_database_code_depnum_ccdc_archive 'CCDC 1823993'
_audit_update_record             
;
2018-02-14 deposited with the CCDC.
2018-04-19 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_CHEMW03_SER_B6_0m           
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: The solvent molecules were highly disordered not all the ones detected by TGA analysis, have been modeled but anyway all the ones detected have been added in final formula.
;
_vrf_PLAT043_SER_B6_0m           
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..     283.60 Check
RESPONSE: The solvent molecules were highly disordered not all the ones detected by TGA analysis, have been modeled but anyway all the ones detected have been added in final formula.
;
_vrf_PLAT234_SER_B6_0m           
;
PROBLEM: Large Hirshfeld Difference O2H      --C1H              0.37 Ang.
RESPONSE: It shoud be related to expected disorder of terminal serine moieties pointing within large pores
;
_vrf_PLAT430_SER_B6_0m           
;
PROBLEM: Short Inter D...A Contact  O2       ..O2W              2.47 Ang.
RESPONSE: short intermolecular contacts between water molecules and the whole network are unavoidable due to the expected severe disorder of solvent. 
;
_vrf_PLAT601_SER_B6_0m           
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of .        220 Ang**3
RESPONSE: The solvent molecules were highly disordered not all the ones detected by TGA analysis, have been modeled but anyway all the ones detected have been added in final formula the quite large channels featured by this series of MOFs likely account for that.  As a consequence, we could  subtract the contribution to the diffraction pattern from the highly disordered water located in the voids from the observed data through the SQUEEZE method, implemented in PLATON. Anyway the reasonable final parameters reached make us confident it could the best ?real? model with voids filled by disordered solvent.
;
_vrf_PLAT939_SER_B6_0m           
;
PROBLEM: Large Value of Not (SHELXL) Weight Optimized S .    4477.08 Check
RESPONSE: It should be related either to intrinsic imperfections (as the presence of large outliers in the data set) quite normal for crystals that suffered a single-crystal to single-crystal process
;
# Added during the CSD deposition process: Wednesday 14 February 2018 10:46 AM
# end Validation Reply Form


_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H89 Ca Cu6 N9 O51'
_chemical_formula_weight         1957.54

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      hexagonal
_space_group_IT_number           173
_space_group_name_H-M_alt        'P 63'
_space_group_name_Hall           'P 6c'

_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, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'

_cell_length_a                   17.9035(9)
_cell_length_b                   17.9035(9)
_cell_length_c                   12.6421(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     3509.3(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    9708
_cell_measurement_theta_min      2.28
_cell_measurement_theta_max      28.0

_exptl_crystal_description       hexagonal-prisms
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.853
_exptl_crystal_F_000             2012
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_absorpt_coefficient_mu    1.980
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.611
_exptl_absorpt_correction_T_max  0.689
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            78211
_diffrn_reflns_av_unetI/netI     0.0174
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.313
_diffrn_reflns_theta_max         28.658
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5995
_reflns_number_gt                5468
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.906
_reflns_Friedel_fraction_max     0.987
_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 APEX'
_computing_cell_refinement       'Bruker APEX'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1106P)²+5.3130P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2430 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.054(8)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5995
_refine_ls_number_parameters     274
_refine_ls_number_restraints     43
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_gt           0.0491
_refine_ls_wR_factor_ref         0.1607
_refine_ls_wR_factor_gt          0.1525
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.050
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.13841(4) 0.58585(4) -0.06557(5) 0.0186(2) Uani 1 1 d . . . . .
Cu2 Cu 0.13743(4) 0.57840(5) 0.19646(5) 0.0215(2) Uani 1 1 d . . . . .
Ca1 Ca 0.3333 0.6667 0.0668(2) 0.0102(3) Uani 1 3 d S T P . .
O1H O 0.1790(2) 0.6426(2) 0.0680(4) 0.0163(6) Uani 1 1 d . . . . .
N1 N 0.0975(4) 0.4964(4) 0.3104(5) 0.0270(12) Uani 1 1 d . . . . .
N2 N 0.0986(4) 0.5095(4) -0.1843(5) 0.0230(11) Uani 1 1 d . . . . .
O1 O 0.2377(3) 0.5636(3) -0.0712(4) 0.0198(8) Uani 1 1 d . . . . .
O2 O 0.0211(3) 0.5776(3) -0.0781(4) 0.0250(10) Uani 1 1 d . . . . .
O3 O 0.2032(4) 0.7123(4) -0.1628(5) 0.0374(14) Uani 1 1 d . . . . .
O4 O 0.2392(3) 0.5611(3) 0.2037(4) 0.0204(9) Uani 1 1 d . . . . .
O5 O 0.2013(3) 0.7027(4) 0.2995(5) 0.0372(14) Uani 1 1 d . . . . .
O6 O 0.0209(3) 0.5698(3) 0.2103(4) 0.0235(10) Uani 1 1 d . . . . .
C1 C 0.2333(4) 0.5127(4) -0.1484(6) 0.0251(14) Uani 1 1 d . . . . .
C2 C -0.0198(4) 0.5273(4) -0.1532(5) 0.0203(11) Uani 1 1 d . . . . .
C3 C 0.1576(4) 0.4806(5) -0.2236(6) 0.0315(16) Uani 1 1 d D . . . .
H3A H 0.1275 0.4166 -0.2323 0.038 Uiso 1 1 calc R U . . .
C4 C 0.2381(4) 0.5133(5) 0.2766(6) 0.0277(15) Uani 1 1 d . . . . .
C5 C 0.1525(6) 0.4644(7) 0.3457(8) 0.046(2) Uani 1 1 d . . . . .
H5A H 0.1671 0.4793 0.4220 0.055 Uiso 1 1 calc R U . . .
C6 C -0.0226(4) 0.5157(4) 0.2844(6) 0.0197(12) Uani 1 1 d . . . . .
C1H C 0.1991(8) 0.5315(14) -0.3375(7) 0.118(8) Uani 1 1 d D . . . .
H1HA H 0.2233 0.5942 -0.3270 0.141 Uiso 1 1 calc R U . . .
H1HB H 0.2469 0.5219 -0.3586 0.141 Uiso 1 1 calc R U . . .
O2H O 0.1378(9) 0.503(2) -0.419(2) 0.33(2) Uani 1 1 d D . . . .
H2HC H 0.1000 0.4515 -0.4087 0.489 Uiso 1 1 calc R U . . .
C2H C 0.1142(7) 0.3658(8) 0.3304(15) 0.084(5) Uani 1 1 d . . . . .
H2HA H 0.1565 0.3496 0.3559 0.101 Uiso 1 1 calc R U . . .
H2HB H 0.0617 0.3347 0.3743 0.101 Uiso 1 1 calc R U . . .
O3H O 0.0933(12) 0.3391(8) 0.2255(18) 0.158(7) Uani 1 1 d . . . . .
H3HA H 0.1387 0.3552 0.1906 0.237 Uiso 1 1 calc R U . . .
O1W O -0.113(3) 0.708(2) 0.096(4) 0.40(3) Uani 1 1 d . U . . .
O2W O -0.0118(4) 0.6469(6) 0.0699(8) 0.083(2) Uani 1 1 d . . . . .
O3W O 0.159(2) 0.7940(12) 0.0654(18) 0.256(14) Uani 1 1 d . . . . .
O4W O -0.0587(9) 0.5657(11) 0.5541(14) 0.150(6) Uani 1 1 d . . . . .
O5W O 0.1241(13) 0.6424(10) 0.5081(14) 0.164(6) Uani 1 1 d . . . . .
O6W O 0.0850(12) 0.7249(16) 0.714(2) 0.268(17) Uani 1 1 d . . . . .
C1B C 0.0874(13) 0.0639(14) 0.405(6) 0.585 Uiso 0.6667 1 d D U P . .
C2B C 0.0235(19) 0.0877(11) 0.403(6) 0.599 Uiso 0.6667 1 d D U P . .
O2B O 0.1615(17) 0.1552(19) 0.401(6) 0.370 Uiso 0.6667 1 d D U P . .
O1B O 0.065(3) 0.241(3) 0.380(5) 0.85(10) Uani 0.6667 1 d D U P . .
C4B C -0.004(3) 0.155(3) 0.401(8) 0.59(9) Uani 0.6667 1 d D U P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N2 1.913(6) . ?
Cu1 O1H 1.917(5) . ?
Cu1 O1 2.007(4) . ?
Cu1 O2 2.037(4) . ?
Cu1 O3 2.314(5) . ?
Cu1 Ca1 3.4675(14) . ?
Cu2 O1H 1.912(5) . ?
Cu2 N1 1.921(6) . ?
Cu2 O4 1.997(4) . ?
Cu2 O6 2.020(4) . ?
Cu2 O5 2.327(6) . ?
Cu2 Ca1 3.4558(14) . ?
Ca1 O4 2.494(5) 3_565 ?
Ca1 O4 2.494(5) . ?
Ca1 O4 2.494(5) 2_665 ?
Ca1 O1 2.494(5) 3_565 ?
Ca1 O1 2.494(5) 2_665 ?
Ca1 O1 2.494(5) . ?
Ca1 O1H 2.574(3) 3_565 ?
Ca1 O1H 2.574(3) 2_665 ?
Ca1 O1H 2.574(3) . ?
Ca1 Cu2 3.4557(14) 2_665 ?
Ca1 Cu2 3.4558(14) 3_565 ?
N1 C2 1.317(8) 4_565 ?
N1 C5 1.436(9) . ?
N2 C6 1.263(8) 4_564 ?
N2 C3 1.475(8) . ?
O1 C1 1.312(8) . ?
O2 C2 1.260(8) . ?
O3 C1 1.231(8) 3_565 ?
O4 C4 1.251(9) . ?
O5 C4 1.246(9) 3_565 ?
O6 C6 1.291(8) . ?
C1 O3 1.231(8) 2_665 ?
C1 C3 1.514(9) . ?
C2 N1 1.317(8) 4_564 ?
C2 C6 1.543(7) 4_564 ?
C3 C1H 1.666(15) . ?
C4 O5 1.246(9) 2_665 ?
C4 C5 1.593(10) . ?
C5 C2H 1.555(17) . ?
C6 N2 1.263(8) 4_565 ?
C6 C2 1.543(7) 4_565 ?
C1H O2H 1.405(18) . ?
C2H O3H 1.40(2) . ?
C1B C2B 1.404(17) 3 ?
C1B C2B 1.406(15) . ?
C1B O2B 1.506(14) . ?
C2B C1B 1.404(17) 2 ?
C2B C4B 1.52(3) . ?
O1B C4B 1.43(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
N2 Cu1 O1H 167.9(2) . . ?
N2 Cu1 O1 83.2(2) . . ?
O1H Cu1 O1 89.84(16) . . ?
N2 Cu1 O2 83.4(2) . . ?
O1H Cu1 O2 102.18(17) . . ?
O1 Cu1 O2 165.04(18) . . ?
N2 Cu1 O3 96.2(3) . . ?
O1H Cu1 O3 94.4(2) . . ?
O1 Cu1 O3 96.6(2) . . ?
O2 Cu1 O3 91.4(2) . . ?
N2 Cu1 Ca1 127.96(17) . . ?
O1H Cu1 Ca1 46.97(10) . . ?
O1 Cu1 Ca1 45.05(13) . . ?
O2 Cu1 Ca1 148.65(14) . . ?
O3 Cu1 Ca1 86.59(14) . . ?
O1H Cu2 N1 168.6(2) . . ?
O1H Cu2 O4 91.19(16) . . ?
N1 Cu2 O4 82.4(2) . . ?
O1H Cu2 O6 101.33(17) . . ?
N1 Cu2 O6 84.3(2) . . ?
O4 Cu2 O6 166.21(19) . . ?
O1H Cu2 O5 92.4(2) . . ?
N1 Cu2 O5 97.4(3) . . ?
O4 Cu2 O5 94.1(2) . . ?
O6 Cu2 O5 91.1(2) . . ?
O1H Cu2 Ca1 47.24(10) . . ?
N1 Cu2 Ca1 127.58(18) . . ?
O4 Cu2 Ca1 45.29(13) . . ?
O6 Cu2 Ca1 148.09(14) . . ?
O5 Cu2 Ca1 85.81(13) . . ?
O4 Ca1 O4 77.15(18) 3_565 . ?
O4 Ca1 O4 77.15(18) 3_565 2_665 ?
O4 Ca1 O4 77.15(18) . 2_665 ?
O4 Ca1 O1 88.35(11) 3_565 3_565 ?
O4 Ca1 O1 139.29(14) . 3_565 ?
O4 Ca1 O1 136.64(14) 2_665 3_565 ?
O4 Ca1 O1 139.29(14) 3_565 2_665 ?
O4 Ca1 O1 136.64(14) . 2_665 ?
O4 Ca1 O1 88.35(11) 2_665 2_665 ?
O1 Ca1 O1 76.47(18) 3_565 2_665 ?
O4 Ca1 O1 136.64(14) 3_565 . ?
O4 Ca1 O1 88.35(11) . . ?
O4 Ca1 O1 139.29(14) 2_665 . ?
O1 Ca1 O1 76.47(18) 3_565 . ?
O1 Ca1 O1 76.47(18) 2_665 . ?
O4 Ca1 O1H 66.88(14) 3_565 3_565 ?
O4 Ca1 O1H 135.65(19) . 3_565 ?
O4 Ca1 O1H 70.43(14) 2_665 3_565 ?
O1 Ca1 O1H 66.30(14) 3_565 3_565 ?
O1 Ca1 O1H 72.43(14) 2_665 3_565 ?
O1 Ca1 O1H 135.77(19) . 3_565 ?
O4 Ca1 O1H 135.65(19) 3_565 2_665 ?
O4 Ca1 O1H 70.43(14) . 2_665 ?
O4 Ca1 O1H 66.88(14) 2_665 2_665 ?
O1 Ca1 O1H 135.76(19) 3_565 2_665 ?
O1 Ca1 O1H 66.30(14) 2_665 2_665 ?
O1 Ca1 O1H 72.43(14) . 2_665 ?
O1H Ca1 O1H 119.996(4) 3_565 2_665 ?
O4 Ca1 O1H 70.43(14) 3_565 . ?
O4 Ca1 O1H 66.88(14) . . ?
O4 Ca1 O1H 135.65(19) 2_665 . ?
O1 Ca1 O1H 72.43(14) 3_565 . ?
O1 Ca1 O1H 135.77(19) 2_665 . ?
O1 Ca1 O1H 66.30(14) . . ?
O1H Ca1 O1H 119.996(3) 3_565 . ?
O1H Ca1 O1H 119.997(4) 2_665 . ?
O4 Ca1 Cu2 105.21(13) 3_565 2_665 ?
O4 Ca1 Cu2 64.69(10) . 2_665 ?
O4 Ca1 Cu2 34.69(9) 2_665 2_665 ?
O1 Ca1 Cu2 155.60(11) 3_565 2_665 ?
O1 Ca1 Cu2 80.15(10) 2_665 2_665 ?
O1 Ca1 Cu2 104.81(10) . 2_665 ?
O1H Ca1 Cu2 100.02(9) 3_565 2_665 ?
O1H Ca1 Cu2 33.05(11) 2_665 2_665 ?
O1H Ca1 Cu2 130.96(11) . 2_665 ?
O4 Ca1 Cu2 64.69(10) 3_565 . ?
O4 Ca1 Cu2 34.69(9) . . ?
O4 Ca1 Cu2 105.21(13) 2_665 . ?
O1 Ca1 Cu2 104.81(10) 3_565 . ?
O1 Ca1 Cu2 155.60(11) 2_665 . ?
O1 Ca1 Cu2 80.15(11) . . ?
O1H Ca1 Cu2 130.96(11) 3_565 . ?
O1H Ca1 Cu2 100.02(9) 2_665 . ?
O1H Ca1 Cu2 33.05(11) . . ?
Cu2 Ca1 Cu2 99.36(5) 2_665 . ?
O4 Ca1 Cu2 34.69(9) 3_565 3_565 ?
O4 Ca1 Cu2 105.21(13) . 3_565 ?
O4 Ca1 Cu2 64.69(10) 2_665 3_565 ?
O1 Ca1 Cu2 80.15(11) 3_565 3_565 ?
O1 Ca1 Cu2 104.81(10) 2_665 3_565 ?
O1 Ca1 Cu2 155.59(11) . 3_565 ?
O1H Ca1 Cu2 33.05(11) 3_565 3_565 ?
O1H Ca1 Cu2 130.96(11) 2_665 3_565 ?
O1H Ca1 Cu2 100.02(9) . 3_565 ?
Cu2 Ca1 Cu2 99.36(5) 2_665 3_565 ?
Cu2 Ca1 Cu2 99.36(5) . 3_565 ?
Cu2 O1H Cu1 119.91(16) . . ?
Cu2 O1H Ca1 99.70(17) . . ?
Cu1 O1H Ca1 100.03(18) . . ?
C2 N1 C5 125.9(7) 4_565 . ?
C2 N1 Cu2 116.0(5) 4_565 . ?
C5 N1 Cu2 118.1(5) . . ?
C6 N2 C3 126.9(6) 4_564 . ?
C6 N2 Cu1 116.8(5) 4_564 . ?
C3 N2 Cu1 116.0(4) . . ?
C1 O1 Cu1 114.4(4) . . ?
C1 O1 Ca1 144.7(4) . . ?
Cu1 O1 Ca1 100.22(17) . . ?
C2 O2 Cu1 108.7(4) . . ?
C1 O3 Cu1 120.7(4) 3_565 . ?
C4 O4 Cu2 115.9(4) . . ?
C4 O4 Ca1 143.4(4) . . ?
Cu2 O4 Ca1 100.02(17) . . ?
C4 O5 Cu2 119.2(5) 3_565 . ?
C6 O6 Cu2 109.5(4) . . ?
O3 C1 O1 123.2(6) 2_665 . ?
O3 C1 C3 119.2(6) 2_665 . ?
O1 C1 C3 117.6(5) . . ?
O2 C2 N1 129.5(6) . 4_564 ?
O2 C2 C6 119.1(5) . 4_564 ?
N1 C2 C6 111.4(5) 4_564 4_564 ?
N2 C3 C1 108.5(5) . . ?
N2 C3 C1H 107.6(7) . . ?
C1 C3 C1H 105.3(6) . . ?
O5 C4 O4 126.2(6) 2_665 . ?
O5 C4 C5 116.3(6) 2_665 . ?
O4 C4 C5 117.5(6) . . ?
N1 C5 C2H 114.4(8) . . ?
N1 C5 C4 105.9(6) . . ?
C2H C5 C4 108.2(8) . . ?
N2 C6 O6 129.3(6) 4_565 . ?
N2 C6 C2 111.9(5) 4_565 4_565 ?
O6 C6 C2 118.8(5) . 4_565 ?
O2H C1H C3 112.5(17) . . ?
O3H C2H C5 113.5(10) . . ?
C2B C1B C2B 120(2) 3 . ?
C2B C1B O2B 145(2) 3 . ?
C2B C1B O2B 94.5(12) . . ?
C1B C2B C1B 120(2) 2 . ?
C1B C2B C4B 89(3) 2 . ?
C1B C2B C4B 151(2) . . ?
O1B C4B C2B 115(3) . . ?

_refine_diff_density_max         1.452
_refine_diff_density_min         -1.271
_refine_diff_density_rms         0.342

_shelxl_version_number           2013-4


_exptl_crystal_recrystallization_method 'slow diffusion'
####################################################################### 
# 
# 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_SeriBupr1_0m
_database_code_depnum_ccdc_archive 'CCDC 1823994'
_audit_update_record             
;
2018-02-14 deposited with the CCDC.
2018-04-19 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_SHFSU01_SeriBupr1_0m        
;
PROBLEM: The absolute value of parameter shift to su ratio > 0.20
RESPONSE: C10L ancd C1T parameters  remain constantly oscillating. It is reasonable due to unavoidable disorder of guest molecules expecially in they terminal fragments.
;
_vrf_PLAT080_SeriBupr1_0m        
;
PROBLEM: Maximum Shift/Error ............................       0.51 Why ?
RESPONSE: C10L ancd C1T parameters  remain constantly oscillating. It is reasonable due to unavoidable disorder of guest molecules expecially in they terminal fragments.
;
_vrf_PLAT213_SeriBupr1_0m        
;
PROBLEM: Atom C1P             has ADP max/min Ratio .....        9.0 prolat
RESPONSE: Unavoidable severe disorder of guest molecules from wich C1P belongs.
;
_vrf_PLAT722_SeriBupr1_0m        
;
PROBLEM: Angle   Calc       86.00, Rep      80(10) Dev...       6.00 Degree
RESPONSE: This molecules is expected to be severely disordered as a consequence of its high thermal motion and has an averaged structure of various geometry and orientation.
;
_vrf_PLAT939_SeriBupr1_0m        
;
PROBLEM: Large Value of Not (SHELXL) Weight Optimized S .     898.78 Check
RESPONSE: It is related to intrinsic imperfections quite normal for crystals that suffered a single-crystal to single-crystal process
;
# Added during the CSD deposition process: Wednesday 14 February 2018 10:46 AM
# end Validation Reply Form


_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C37 H90 Ca Cl Cu6 N7 O50'
_chemical_formula_weight         1889.92

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.2262 0.3064 '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'

_space_group_crystal_system      hexagonal
_space_group_IT_number           173
_space_group_name_H-M_alt        'P 63'
_space_group_name_Hall           'P 6c'

_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, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'

_cell_length_a                   17.997(3)
_cell_length_b                   17.997(3)
_cell_length_c                   12.861(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     3607.6(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    6597
_cell_measurement_theta_min      2.26
_cell_measurement_theta_max      24.51

_exptl_crystal_description       hexagonal-prisms
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.740
_exptl_crystal_F_000             1944
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_exptl_absorpt_coefficient_mu    1.957
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.611
_exptl_absorpt_correction_T_max  0.752
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            41906
_diffrn_reflns_av_unetI/netI     0.0742
_diffrn_reflns_av_R_equivalents  0.0775
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.306
_diffrn_reflns_theta_max         30.272
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             7026
_reflns_number_gt                4516
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.882
_reflns_Friedel_fraction_max     0.952
_reflns_Friedel_fraction_full    0.986

_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 APEX'
_computing_cell_refinement       'Bruker APEX'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1267P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1649 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.14(2)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         7026
_refine_ls_number_parameters     380
_refine_ls_number_restraints     250
_refine_ls_R_factor_all          0.1091
_refine_ls_R_factor_gt           0.0612
_refine_ls_wR_factor_ref         0.2015
_refine_ls_wR_factor_gt          0.1693
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_restrained_S_all      1.401
_refine_ls_shift/su_max          0.510
_refine_ls_shift/su_mean         0.026

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 0.42304(6) -0.13571(6) 0.4911(9) 0.0253(3) Uani 1 1 d . . . . .
Cu2 Cu 0.41731(6) -0.13661(6) 0.7478(9) 0.0242(3) Uani 1 1 d . . . . .
Ca1 Ca 0.3333 -0.3333 0.6190(9) 0.0127(4) Uani 1 3 d S T P . .
O1H O 0.3580(3) -0.1779(2) 0.6172(11) 0.0215(8) Uani 1 1 d . . . . .
N1 N 0.5025(6) -0.0970(6) 0.3773(12) 0.035(2) Uani 1 1 d . . . . .
N2 N 0.4922(6) -0.0991(5) 0.8667(11) 0.0282(19) Uani 1 1 d . . . . .
O1 O 0.4394(4) -0.2381(4) 0.4839(10) 0.0248(14) Uani 1 1 d . . . . .
O2 O 0.4303(4) -0.0186(4) 0.4759(11) 0.0299(17) Uani 1 1 d . . . . .
O3 O 0.2977(5) -0.2021(4) 0.3864(11) 0.042(2) Uani 1 1 d . . . . .
O4 O 0.4371(4) -0.2381(3) 0.7554(10) 0.0236(14) Uani 1 1 d . . . . .
O5 O 0.4262(4) -0.0201(4) 0.7642(11) 0.0319(18) Uani 1 1 d . . . . .
O6 O 0.2896(5) -0.2014(5) 0.8425(11) 0.042(2) Uani 1 1 d . . . . .
C1 C 0.4873(7) -0.2376(6) 0.4125(13) 0.031(2) Uani 1 1 d . . . . .
C2 C 0.5311(9) -0.1562(8) 0.3358(15) 0.054(4) Uani 1 1 d . . . . .
C3 C 0.4823(6) 0.0217(6) 0.3987(13) 0.026(2) Uani 1 1 d . . . . .
C4 C 0.4869(7) -0.2332(6) 0.8331(13) 0.030(2) Uani 1 1 d . . . . .
C5 C 0.5219(9) -0.1555(7) 0.9012(14) 0.047(3) Uani 1 1 d . . . . .
C6 C 0.4750(6) 0.0208(6) 0.8401(12) 0.026(2) Uani 1 1 d . . . . .
C2H C 0.4798(12) -0.1939(9) 1.0191(14) 0.073(4) Uani 1 1 d . . . . .
C3H C 0.6319(10) -0.1138(8) 0.353(2) 0.087(6) Uani 1 1 d . . . . .
O2H O 0.4003(14) -0.2270(14) 1.0367(19) 0.121(7) Uani 0.7 1 d . . P . .
O2H' O 0.488(2) -0.1451(14) 1.097(2) 0.064(9) Uani 0.3 1 d . . P . .
O3H O 0.6607(8) -0.0918(11) 0.461(2) 0.171(8) Uani 1 1 d . . . . .
O2W O 0.6532(9) -0.0178(7) 0.1177(17) 0.122(4) Uani 1 1 d . . . . .
O3W O 0.7194(13) 0.0818(9) 0.4655(17) 0.181(9) Uani 1 1 d . . . . .
O4W O 0.751(5) 0.001(5) -0.205(6) 0.54(4) Uiso 1 1 d . . . . .
O5W O 0.679(3) -0.149(3) 0.091(3) 0.38(2) Uani 1 1 d . U . . .
O6W O 0.6456(12) 0.1311(11) 0.6804(15) 0.172(9) Uani 1 1 d . U . . .
C2T C 1.0000 0.0000 0.019(3) 1.00(9) Uani 1 3 d DS TU P . .
C10L C 0.999(3) 0.146(4) 0.044(7) 0.86(9) Uani 0.3333 1 d D U P . .
N1L N 0.8976(19) 0.011(3) -0.068(2) 0.97(9) Uani 0.3333 1 d D U P . .
C6L C 0.907(2) 0.077(2) 0.0145(19) 0.92(9) Uani 0.3333 1 d D U P . .
C4T C 0.898(2) -0.1137(15) -0.068(3) 0.98(9) Uani 0.3333 1 d D U P . .
C1O C 0.882(6) 0.044(3) 0.127(2) 0.87(9) Uani 0.3333 1 d D U P . .
C3T C 1.0000 0.0000 -0.155(3) 0.99(9) Uani 1 3 d DS TU P . .
C1T C 0.9486(10) -0.0259(15) -0.068(3) 0.98(9) Uani 0.3333 1 d D U P . .
O10 O 0.899(7) -0.013(6) 0.134(7) 0.83(9) Uani 0.3333 1 d D U P . .
C1P C 0.835(6) 0.104(4) 0.255(4) 1.22(10) Uani 0.3333 1 d DG U P . .
C3P C 0.832(7) 0.170(4) 0.309(5) 1.22(10) Uani 0.3333 1 d G U P . .
C2P C 0.870(6) 0.252(4) 0.267(4) 1.21(10) Uani 0.3333 1 d G U P . .
C4P C 0.909(3) 0.268(3) 0.170(4) 1.21(10) Uani 0.3333 1 d DG U P . .
C5P C 0.912(5) 0.203(3) 0.116(4) 1.22(10) Uani 0.3333 1 d DG U P . .
C6P C 0.875(6) 0.121(3) 0.158(4) 1.23(10) Uani 0.3333 1 d DG U P . .
Cl1 Cl 0.953(4) 0.378(3) 0.129(5) 0.37(3) Uani 0.3333 1 d D U P . .
O7W O 0.8024(10) 0.1745(12) 0.115(2) 0.100(5) Uani 0.6667 1 d . U P . .
O8W O 0.9495(8) 0.3767(9) 0.1250(17) 0.065(5) Uani 0.6667 1 d . U P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O1H 1.920(8) . ?
Cu1 N1 1.918(9) . ?
Cu1 O1 2.009(6) . ?
Cu1 O2 2.055(6) . ?
Cu1 Cl1 2.98(6) 6_545 ?
Cu1 O3 2.373(8) . ?
Cu1 Ca1 3.495(2) . ?
Cu2 N2 1.923(8) . ?
Cu2 O1H 1.929(8) . ?
Cu2 O4 2.031(5) . ?
Cu2 O5 2.032(6) . ?
Cu2 C2P 3.56(19) 6_545 ?
Cu2 O6 2.333(8) . ?
Cu2 Cl1 2.91(4) 6_545 ?
Cu2 Ca1 3.495(2) . ?
Ca1 O1 2.516(7) 3_655 ?
Ca1 O1 2.516(7) . ?
Ca1 O1 2.516(7) 2_545 ?
Ca1 O4 2.510(7) 2_545 ?
Ca1 O4 2.510(7) 3_655 ?
Ca1 O4 2.510(7) . ?
Ca1 O1H 2.604(4) 3_655 ?
Ca1 O1H 2.604(4) . ?
Ca1 O1H 2.604(4) 2_545 ?
Ca1 Cu1 3.495(2) 2_545 ?
Ca1 Cu1 3.495(2) 3_655 ?
N1 C6 1.311(13) 4_654 ?
N1 C2 1.494(13) . ?
N2 C3 1.297(12) 4_655 ?
N2 C5 1.434(14) . ?
N2 C2P 2.89(18) 6_545 ?
O1 C1 1.256(12) . ?
O2 C3 1.308(12) . ?
O3 C1 1.261(12) 2_545 ?
O4 C4 1.316(12) . ?
O5 C6 1.273(11) . ?
O6 C4 1.267(12) 2_545 ?
C1 O3 1.261(12) 3_655 ?
C1 C2 1.607(15) . ?
C2 C3H 1.59(2) . ?
C3 N2 1.297(12) 4_654 ?
C3 C6 1.527(10) 4_654 ?
C4 O6 1.267(12) 3_655 ?
C4 C5 1.496(15) . ?
C4 C3P 2.8(3) 6_545 ?
C5 C2H 1.68(2) . ?
C5 C3P 2.90(18) 6_545 ?
C6 N1 1.311(13) 4_655 ?
C6 C3 1.527(10) 4_655 ?
C2H O2H 1.27(2) . ?
C2H O2H' 1.29(3) . ?
C3H O3H 1.46(3) . ?
O2H O2H' 1.72(4) . ?
O3H C5P 2.16(15) 6_545 ?
C2T C1T 1.378(13) . ?
C2T C1T 1.378(13) 3_765 ?
C2T C1T 1.378(13) 2_645 ?
C10L C6L 1.5400(15) . ?
N1L C1T 1.373(13) . ?
N1L C6L 1.5400(15) . ?
C6L C1O 1.5400(15) . ?
C4T C1T 1.374(13) . ?
C1O O10 1.201(14) . ?
C1O C6P 1.512(10) . ?
C3T C1T 1.379(13) . ?
C3T C1T 1.379(13) 3_765 ?
C3T C1T 1.379(13) 2_645 ?
C1T C1T 1.39(3) 3_765 ?
C1T C1T 1.39(3) 2_645 ?
C1P C3P 1.3900 . ?
C1P C6P 1.3900 . ?
C1P O7W 2.43(8) . ?
C3P C2P 1.3900 . ?
C3P C4 2.79(8) 5_664 ?
C3P C5 2.90(6) 5_664 ?
C2P C4P 1.3900 . ?
C2P N2 2.89(5) 5_664 ?
C2P Cu2 3.56(6) 5_664 ?
C4P O8W 1.80(6) . ?
C4P C5P 1.3900 . ?
C4P Cl1 1.797(14) . ?
C5P C6P 1.3900 . ?
C5P O8W 2.85(5) . ?
C5P O3H 2.16(6) 5_664 ?
C6P O7W 2.05(8) . ?
Cl1 O8W 0.08(7) . ?
Cl1 Cu1 2.98(6) 5_664 ?
Cl1 Cu2 2.91(4) 5_664 ?

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
O1H Cu1 N1 169.9(3) . . ?
O1H Cu1 O1 90.9(2) . . ?
N1 Cu1 O1 82.7(3) . . ?
O1H Cu1 O2 101.5(2) . . ?
N1 Cu1 O2 84.4(3) . . ?
O1 Cu1 O2 166.8(3) . . ?
O1H Cu1 Cl1 85.8(9) . 6_545 ?
N1 Cu1 Cl1 86.5(10) . 6_545 ?
O1 Cu1 Cl1 90.2(10) . 6_545 ?
O2 Cu1 Cl1 86.3(11) . 6_545 ?
O1H Cu1 O3 92.4(3) . . ?
N1 Cu1 O3 95.6(4) . . ?
O1 Cu1 O3 92.9(3) . . ?
O2 Cu1 O3 91.1(3) . . ?
Cl1 Cu1 O3 176.5(9) 6_545 . ?
O1H Cu1 Ca1 47.17(13) . . ?
N1 Cu1 Ca1 127.6(2) . . ?
O1 Cu1 Ca1 45.0(2) . . ?
O2 Cu1 Ca1 148.0(2) . . ?
Cl1 Cu1 Ca1 95.8(11) 6_545 . ?
O3 Cu1 Ca1 85.17(18) . . ?
N2 Cu2 O1H 169.4(3) . . ?
N2 Cu2 O4 82.6(3) . . ?
O1H Cu2 O4 90.4(2) . . ?
N2 Cu2 O5 82.8(3) . . ?
O1H Cu2 O5 103.4(2) . . ?
O4 Cu2 O5 164.7(3) . . ?
N2 Cu2 C2P 54(5) . 6_545 ?
O1H Cu2 C2P 115(5) . 6_545 ?
O4 Cu2 C2P 53(7) . 6_545 ?
O5 Cu2 C2P 114(7) . 6_545 ?
N2 Cu2 O6 95.9(4) . . ?
O1H Cu2 O6 92.6(3) . . ?
O4 Cu2 O6 95.5(3) . . ?
O5 Cu2 O6 90.7(3) . . ?
C2P Cu2 O6 135.1(18) 6_545 . ?
N2 Cu2 Cl1 84.4(12) . 6_545 ?
O1H Cu2 Cl1 87.5(12) . 6_545 ?
O4 Cu2 Cl1 87.9(10) . 6_545 ?
O5 Cu2 Cl1 86.0(11) . 6_545 ?
C2P Cu2 Cl1 47(2) 6_545 6_545 ?
O6 Cu2 Cl1 176.6(10) . 6_545 ?
N2 Cu2 Ca1 127.2(3) . . ?
O1H Cu2 Ca1 47.23(13) . . ?
O4 Cu2 Ca1 44.99(18) . . ?
O5 Cu2 Ca1 149.9(2) . . ?
C2P Cu2 Ca1 89(8) 6_545 . ?
O6 Cu2 Ca1 85.52(19) . . ?
Cl1 Cu2 Ca1 97.0(11) 6_545 . ?
O1 Ca1 O1 77.6(2) 3_655 . ?
O1 Ca1 O1 77.6(2) 3_655 2_545 ?
O1 Ca1 O1 77.6(2) . 2_545 ?
O1 Ca1 O4 137.1(2) 3_655 2_545 ?
O1 Ca1 O4 138.6(2) . 2_545 ?
O1 Ca1 O4 88.02(14) 2_545 2_545 ?
O1 Ca1 O4 88.03(14) 3_655 3_655 ?
O1 Ca1 O4 137.1(2) . 3_655 ?
O1 Ca1 O4 138.6(2) 2_545 3_655 ?
O4 Ca1 O4 76.5(3) 2_545 3_655 ?
O1 Ca1 O4 138.6(2) 3_655 . ?
O1 Ca1 O4 88.02(14) . . ?
O1 Ca1 O4 137.1(2) 2_545 . ?
O4 Ca1 O4 76.5(3) 2_545 . ?
O4 Ca1 O4 76.5(3) 3_655 . ?
O1 Ca1 O1H 66.3(2) 3_655 3_655 ?
O1 Ca1 O1H 70.6(2) . 3_655 ?
O1 Ca1 O1H 135.7(3) 2_545 3_655 ?
O4 Ca1 O1H 136.0(3) 2_545 3_655 ?
O4 Ca1 O1H 66.6(2) 3_655 3_655 ?
O4 Ca1 O1H 72.3(2) . 3_655 ?
O1 Ca1 O1H 135.7(3) 3_655 . ?
O1 Ca1 O1H 66.3(2) . . ?
O1 Ca1 O1H 70.6(2) 2_545 . ?
O4 Ca1 O1H 72.3(2) 2_545 . ?
O4 Ca1 O1H 136.0(3) 3_655 . ?
O4 Ca1 O1H 66.6(2) . . ?
O1H Ca1 O1H 119.992(8) 3_655 . ?
O1 Ca1 O1H 70.6(2) 3_655 2_545 ?
O1 Ca1 O1H 135.7(3) . 2_545 ?
O1 Ca1 O1H 66.3(2) 2_545 2_545 ?
O4 Ca1 O1H 66.6(2) 2_545 2_545 ?
O4 Ca1 O1H 72.3(2) 3_655 2_545 ?
O4 Ca1 O1H 136.0(3) . 2_545 ?
O1H Ca1 O1H 119.995(7) 3_655 2_545 ?
O1H Ca1 O1H 119.990(7) . 2_545 ?
O1 Ca1 Cu1 105.57(19) 3_655 . ?
O1 Ca1 Cu1 34.40(13) . . ?
O1 Ca1 Cu1 65.30(14) 2_545 . ?
O4 Ca1 Cu1 104.41(14) 2_545 . ?
O4 Ca1 Cu1 155.64(16) 3_655 . ?
O4 Ca1 Cu1 80.02(14) . . ?
O1H Ca1 Cu1 99.93(13) 3_655 . ?
O1H Ca1 Cu1 32.74(17) . . ?
O1H Ca1 Cu1 131.01(16) 2_545 . ?
O1 Ca1 Cu1 65.29(14) 3_655 2_545 ?
O1 Ca1 Cu1 105.57(19) . 2_545 ?
O1 Ca1 Cu1 34.40(13) 2_545 2_545 ?
O4 Ca1 Cu1 80.02(14) 2_545 2_545 ?
O4 Ca1 Cu1 104.40(14) 3_655 2_545 ?
O4 Ca1 Cu1 155.64(16) . 2_545 ?
O1H Ca1 Cu1 131.01(16) 3_655 2_545 ?
O1H Ca1 Cu1 99.93(13) . 2_545 ?
O1H Ca1 Cu1 32.74(17) 2_545 2_545 ?
Cu1 Ca1 Cu1 99.67(9) . 2_545 ?
O1 Ca1 Cu1 34.40(13) 3_655 3_655 ?
O1 Ca1 Cu1 65.29(14) . 3_655 ?
O1 Ca1 Cu1 105.57(19) 2_545 3_655 ?
O4 Ca1 Cu1 155.64(16) 2_545 3_655 ?
O4 Ca1 Cu1 80.02(14) 3_655 3_655 ?
O4 Ca1 Cu1 104.40(14) . 3_655 ?
O1H Ca1 Cu1 32.74(17) 3_655 3_655 ?
O1H Ca1 Cu1 131.01(16) . 3_655 ?
O1H Ca1 Cu1 99.93(13) 2_545 3_655 ?
Cu1 Ca1 Cu1 99.67(9) . 3_655 ?
Cu1 Ca1 Cu1 99.67(9) 2_545 3_655 ?
Cu2 O1H Cu1 118.2(2) . . ?
Cu2 O1H Ca1 99.8(3) . . ?
Cu1 O1H Ca1 100.1(2) . . ?
C6 N1 C2 125.4(9) 4_654 . ?
C6 N1 Cu1 116.3(7) 4_654 . ?
C2 N1 Cu1 118.3(7) . . ?
C3 N2 C5 127.3(9) 4_655 . ?
C3 N2 Cu2 116.0(7) 4_655 . ?
C5 N2 Cu2 116.2(7) . . ?
C3 N2 C2P 117(9) 4_655 6_545 ?
C5 N2 C2P 53(2) . 6_545 ?
Cu2 N2 C2P 93(7) . 6_545 ?
C1 O1 Cu1 116.2(6) . . ?
C1 O1 Ca1 142.6(6) . . ?
Cu1 O1 Ca1 100.6(3) . . ?
C3 O2 Cu1 107.5(6) . . ?
C1 O3 Cu1 118.6(7) 2_545 . ?
C4 O4 Cu2 113.3(6) . . ?
C4 O4 Ca1 145.7(6) . . ?
Cu2 O4 Ca1 100.1(2) . . ?
C6 O5 Cu2 110.7(6) . . ?
C4 O6 Cu2 123.2(6) 2_545 . ?
O3 C1 O1 127.5(9) 3_655 . ?
O3 C1 C2 113.7(9) 3_655 . ?
O1 C1 C2 118.5(9) . . ?
N1 C2 C3H 108.9(11) . . ?
N1 C2 C1 104.1(9) . . ?
C3H C2 C1 105.9(10) . . ?
O2 C3 N2 127.4(9) . 4_654 ?
O2 C3 C6 119.9(6) . 4_654 ?
N2 C3 C6 112.7(8) 4_654 4_654 ?
O6 C4 O4 119.6(9) 3_655 . ?
O6 C4 C5 122.6(9) 3_655 . ?
O4 C4 C5 117.5(8) . . ?
O6 C4 C3P 67(7) 3_655 6_545 ?
O4 C4 C3P 122(2) . 6_545 ?
C5 C4 C3P 79(9) . 6_545 ?
N2 C5 C4 110.4(9) . . ?
N2 C5 C2H 108.7(11) . . ?
C4 C5 C2H 104.5(10) . . ?
N2 C5 C3P 125(4) . 6_545 ?
C4 C5 C3P 71(9) . 6_545 ?
C2H C5 C3P 124.6(17) . 6_545 ?
O5 C6 N1 130.4(9) . 4_655 ?
O5 C6 C3 117.6(7) . 4_655 ?
N1 C6 C3 112.0(7) 4_655 4_655 ?
O2H C2H O2H' 84(2) . . ?
O2H C2H C5 121.7(15) . . ?
O2H' C2H C5 123.1(15) . . ?
O3H C3H C2 115.2(12) . . ?
C2H O2H O2H' 48.4(14) . . ?
C2H O2H' O2H 47.2(13) . . ?
C3H O3H C5P 165(7) . 6_545 ?
C1T C2T C1T 60.5(11) . 3_765 ?
C1T C2T C1T 60.5(11) . 2_645 ?
C1T C2T C1T 60.5(11) 3_765 2_645 ?
C1T N1L C6L 121.8(17) . . ?
N1L C6L C10L 116.9(7) . . ?
N1L C6L C1O 116.9(7) . . ?
C10L C6L C1O 94.0(8) . . ?
O10 C1O C6P 158(9) . . ?
O10 C1O C6L 104(2) . . ?
C6P C1O C6L 92(2) . . ?
C1T C3T C1T 60.4(11) . 3_765 ?
C1T C3T C1T 60.4(11) . 2_645 ?
C1T C3T C1T 60.4(11) 3_765 2_645 ?
C4T C1T C2T 109.6(13) . . ?
C4T C1T C3T 109.5(13) . . ?
C2T C1T C3T 108.9(13) . . ?
C4T C1T N1L 109.7(13) . . ?
C2T C1T N1L 109.6(13) . . ?
C3T C1T N1L 109.5(13) . . ?
C4T C1T C1T 155.1(17) . 3_765 ?
C2T C1T C1T 59.8(6) . 3_765 ?
C3T C1T C1T 59.8(6) . 3_765 ?
N1L C1T C1T 95.2(17) . 3_765 ?
C4T C1T C1T 95.1(17) . 2_645 ?
C2T C1T C1T 59.8(6) . 2_645 ?
C3T C1T C1T 59.8(6) . 2_645 ?
N1L C1T C1T 155.2(17) . 2_645 ?
C1T C1T C1T 59.999(3) 3_765 2_645 ?
C3P C1P C6P 120.0 . . ?
C3P C1P O7W 79(2) . . ?
C6P C1P O7W 57(3) . . ?
C2P C3P C1P 120.0 . . ?
C2P C3P C4 55.8(18) . 5_664 ?
C1P C3P C4 150(4) . 5_664 ?
C2P C3P C5 52.0(17) . 5_664 ?
C1P C3P C5 172(2) . 5_664 ?
C4 C3P C5 30.4(7) 5_664 5_664 ?
C4P C2P C3P 120.0 . . ?
C4P C2P N2 111(2) . 5_664 ?
C3P C2P N2 128.3(19) . 5_664 ?
C4P C2P Cu2 89.6(16) . 5_664 ?
C3P C2P Cu2 146.6(16) . 5_664 ?
N2 C2P Cu2 32.6(7) 5_664 5_664 ?
O8W C4P C5P 126(2) . . ?
O8W C4P C2P 114(2) . . ?
C5P C4P C2P 120.0 . . ?
O8W C4P Cl1 3(2) . . ?
C5P C4P Cl1 126.6(15) . . ?
C2P C4P Cl1 113.4(15) . . ?
C4P C5P C6P 120.0 . . ?
C4P C5P O8W 30.8(15) . . ?
C6P C5P O8W 150.7(15) . . ?
C4P C5P O3H 97.4(19) . 5_664 ?
C6P C5P O3H 132(2) . 5_664 ?
O8W C5P O3H 70.5(14) . 5_664 ?
C5P C6P C1P 120.0 . . ?
C5P C6P C1O 131.1(10) . . ?
C1P C6P C1O 108.0(9) . . ?
C5P C6P O7W 59(2) . . ?
C1P C6P O7W 88(3) . . ?
C1O C6P O7W 137(6) . . ?
O8W Cl1 C4P 94(10) . . ?
O8W Cl1 Cu1 32(10) . 5_664 ?
C4P Cl1 Cu1 125(2) . 5_664 ?
O8W Cl1 Cu2 80(10) . 5_664 ?
C4P Cl1 Cu2 106(2) . 5_664 ?
Cu1 Cl1 Cu2 68.3(10) 5_664 5_664 ?
C6P O7W C1P 34.9(13) . . ?
C4P O8W Cl1 84(10) . . ?
C4P O8W C5P 23.2(9) . . ?
Cl1 O8W C5P 89(10) . . ?

_refine_diff_density_max         1.157
_refine_diff_density_min         -1.502
_refine_diff_density_rms         0.314

_shelxl_version_number           2013-4


_exptl_crystal_recrystallization_method 'slow diffusion'
