# Electronic Supplementary Material (ESI) for Materials Chemistry Frontiers.
# This journal is © the Partner Organisations 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_c:FJI-C3
_database_code_depnum_ccdc_archive 'CCDC 1444652'
_audit_update_record             
;
2016-01-19 deposited with the CCDC.
2018-03-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C31 H26 Cu3 N1 O15 P2'
_chemical_formula_weight         905.09

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'

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

_cell_length_a                   12.86130(10)
_cell_length_b                   18.9007(2)
_cell_length_c                   20.5254(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.9910(10)
_cell_angle_gamma                90.00
_cell_volume                     4861.77(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    17959
_cell_measurement_theta_min      3.2270
_cell_measurement_theta_max      76.3640

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1824
_exptl_absorpt_coefficient_mu    2.609
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7991
_exptl_absorpt_correction_T_max  0.9497
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger.

The calculated free volume of FJI-C3 with removal of guest solvent molecules  is 48.5% by PLATON (1.8 Angstrom probe radius). We employed 
PLATON SQUEEZE to calculate the contribution to the contribution to the diffraction 
from the solvent region and thereby produced a set of solvent-free diffraction intensities. 
The final formula was calculated from  TGA and with elemental analysis data.
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.5594
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            35311
_diffrn_reflns_av_R_equivalents  0.0334
_diffrn_reflns_av_sigmaI/netI    0.0279
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         3.22
_diffrn_reflns_theta_max         76.63
_reflns_number_total             10108
_reflns_number_gt                8917
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0585P)²+14.2345P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10108
_refine_ls_number_parameters     436
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0457
_refine_ls_wR_factor_ref         0.1227
_refine_ls_wR_factor_gt          0.1203
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_restrained_S_all      1.018
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.08531(3) 0.501534(19) -0.267689(17) 0.00587(10) Uani 1 1 d . . .
Cu2 Cu -0.09077(3) 0.529307(19) -0.228308(17) 0.00575(9) Uani 1 1 d . . .
Cu3 Cu 0.51168(3) 0.46645(2) 0.253592(18) 0.00934(10) Uani 1 1 d . . .
P4 P 0.20063(5) 0.94568(3) -0.16151(3) 0.00637(13) Uani 1 1 d . . .
P5 P 0.30355(5) 0.41402(3) 0.15747(3) 0.00621(13) Uani 1 1 d . . .
O12 O 0.39901(4) 0.46781(4) 0.30457(3) 0.0195(4) Uani 1 1 d . . .
H12A H 0.3455 0.4441 0.2838 0.029 Uiso 1 1 d R . .
H12B H 0.3800 0.5104 0.3089 0.029 Uiso 1 1 d R . .
O1 O 0.13462(4) 0.59591(4) -0.23494(3) 0.0141(4) Uani 1 1 d R . .
O2 O -0.02390(4) 0.62282(4) -0.21341(3) 0.0146(4) Uani 1 1 d R . .
O15 O 0.50751(7) 0.08799(4) 0.20661(5) 0.0163(4) Uani 1 1 d R . .
O3 O -0.00262(4) 0.49353(4) -0.14189(3) 0.0150(4) Uani 1 1 d R . .
O11 O 0.61868(5) 0.47517(3) 0.20001(4) 0.0165(4) Uani 1 1 d R . .
H11A H 0.6156 0.5169 0.1805 0.025 Uiso 1 1 d R . .
H11B H 0.6096 0.4429 0.1682 0.025 Uiso 1 1 d R . .
O8 O 0.50920(6) 0.95385(4) 0.14824(4) 0.0151(4) Uani 1 1 d R . .
O4 O 0.14203(4) 0.46520(4) -0.17761(3) 0.0149(4) Uani 1 1 d R . .
O14 O 0.36491(7) 0.06839(4) 0.24796(5) 0.0150(4) Uani 1 1 d R . .
C18 C 0.06881(4) 0.63860(4) -0.21874(3) 0.0095(5) Uani 1 1 d R . .
C25 C 0.26319(5) 0.93911(3) -0.07342(3) 0.0085(5) Uani 1 1 d R . .
O7 O 0.35301(6) 0.94685(3) 0.17600(4) 0.0152(4) Uani 1 1 d R . .
C13 C 0.26946(6) 0.27995(3) 0.20499(4) 0.0117(5) Uani 1 1 d R . .
H13 H 0.2096 0.3000 0.2182 0.014 Uiso 1 1 calc R . .
C19 C 0.1018(2) 0.71446(14) -0.20647(13) 0.0097(5) Uani 1 1 d . . .
C4 C 0.1314(2) 0.42237(14) 0.04927(13) 0.0110(5) Uani 1 1 d . . .
H4 H 0.0893 0.4114 0.0805 0.013 Uiso 1 1 calc R . .
C8 C 0.3295(2) 0.32102(14) 0.17098(12) 0.0086(5) Uani 1 1 d . . .
C11 C 0.3855(2) 0.18029(14) 0.20083(13) 0.0098(5) Uani 1 1 d . . .
C6 C 0.3040(2) 0.43683(15) 0.02345(14) 0.0125(5) Uani 1 1 d . . .
H6 H 0.3796 0.4369 0.0374 0.015 Uiso 1 1 calc R . .
C14 C 0.4217(2) 0.10621(14) 0.21987(12) 0.0094(5) Uani 1 1 d . . .
C26 C 0.1992(2) 0.93558(15) -0.02602(14) 0.0138(5) Uani 1 1 d . . .
H26 H 0.1237 0.9354 -0.0403 0.017 Uiso 1 1 calc R . .
C22 C 0.1600(2) 0.85595(14) -0.18391(13) 0.0091(5) Uani 1 1 d . . .
C20 C 0.2012(2) 0.73767(14) -0.21514(14) 0.0127(5) Uani 1 1 d . . .
H20 H 0.2488 0.7053 -0.2286 0.015 Uiso 1 1 calc R . .
C3 C 0.0823(2) 0.43594(14) -0.01716(13) 0.0110(5) Uani 1 1 d . . .
H3 H 0.0066 0.4353 -0.0311 0.013 Uiso 1 1 calc R . .
C5 C 0.2421(2) 0.42483(13) 0.07008(12) 0.0083(5) Uani 1 1 d . . .
C28 C 0.3581(2) 0.93391(14) 0.06234(13) 0.0098(5) Uani 1 1 d . . .
C21 C 0.2297(2) 0.80800(15) -0.20396(14) 0.0125(5) Uani 1 1 d . . .
H21 H 0.2971 0.8238 -0.2099 0.015 Uiso 1 1 calc R . .
C1 C 0.0908(2) 0.47095(13) -0.13402(12) 0.0090(5) Uani 1 1 d . . .
C31 C 0.4097(2) 0.94410(13) 0.13485(13) 0.0094(5) Uani 1 1 d . . .
C30 C 0.3736(2) 0.93539(14) -0.05247(13) 0.0101(5) Uani 1 1 d . . .
H30 H 0.4167 0.9344 -0.0845 0.012 Uiso 1 1 calc R . .
C7 C 0.2553(2) 0.44876(15) -0.04358(13) 0.0132(5) Uani 1 1 d . . .
H7 H 0.2974 0.4557 -0.0756 0.016 Uiso 1 1 calc R . .
C29 C 0.4208(2) 0.93317(14) 0.01524(13) 0.0104(5) Uani 1 1 d . . .
H29 H 0.4963 0.9311 0.0295 0.013 Uiso 1 1 calc R . .
C10 C 0.4447(2) 0.22177(14) 0.16560(13) 0.0110(5) Uani 1 1 d . . .
H10 H 0.5045 0.2019 0.1522 0.013 Uiso 1 1 calc R . .
C24 C 0.0322(2) 0.76210(15) -0.18674(15) 0.0159(6) Uani 1 1 d . . .
H24 H -0.0352 0.7463 -0.1809 0.019 Uiso 1 1 calc R . .
C9 C 0.4167(2) 0.29149(15) 0.15016(13) 0.0117(5) Uani 1 1 d . . .
H9 H 0.4562 0.3192 0.1256 0.014 Uiso 1 1 calc R . .
C2 C 0.1439(2) 0.45037(14) -0.06301(12) 0.0095(5) Uani 1 1 d . . .
C27 C 0.2467(2) 0.93240(15) 0.04083(13) 0.0126(5) Uani 1 1 d . . .
H27 H 0.2037 0.9291 0.0728 0.015 Uiso 1 1 calc R . .
C12 C 0.2969(2) 0.20901(14) 0.21998(14) 0.0118(5) Uani 1 1 d . . .
H12 H 0.2555 0.1808 0.2429 0.014 Uiso 1 1 calc R . .
C23 C 0.0608(2) 0.83249(15) -0.17562(15) 0.0154(5) Uani 1 1 d . . .
H23 H 0.0130 0.8648 -0.1623 0.018 Uiso 1 1 calc R . .
O6 O 0.27995(14) 0.96970(10) -0.20016(9) 0.0100(4) Uani 1 1 d . . .
O9 O 0.22925(14) 0.43842(10) 0.19939(9) 0.0090(4) Uani 1 1 d . . .
O5 O 0.10140(14) 0.99046(10) -0.16801(9) 0.0100(4) Uani 1 1 d . . .
O10 O 0.41134(14) 0.45034(10) 0.16927(9) 0.0096(4) Uani 1 1 d . . .
O13 O 0.56506(18) 0.35491(11) 0.29186(11) 0.0212(4) Uani 1 1 d . . .
N1 N 0.5294(2) 0.25489(15) 0.34590(14) 0.0237(6) Uani 1 1 d . . .
C15 C 0.5052(3) 0.31866(17) 0.31883(15) 0.0225(6) Uani 1 1 d . . .
C17 C 0.4551(3) 0.21739(19) 0.37780(18) 0.0309(8) Uani 1 1 d . . .
H17C H 0.4886 0.2092 0.4250 0.046 Uiso 1 1 calc R . .
H17B H 0.4363 0.1719 0.3554 0.046 Uiso 1 1 calc R . .
H17A H 0.3905 0.2459 0.3745 0.046 Uiso 1 1 calc R . .
C16 C 0.6303(3) 0.22105(18) 0.34603(18) 0.0295(7) Uani 1 1 d . . .
H16C H 0.6720 0.2511 0.3225 0.044 Uiso 1 1 calc R . .
H16A H 0.6174 0.1752 0.3235 0.044 Uiso 1 1 calc R . .
H16B H 0.6700 0.2140 0.3923 0.044 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O4 1.9535 . ?
Cu1 O1 1.9606 . ?
Cu1 O8 1.9717 4_575 ?
Cu1 O15 1.9761 4_565 ?
Cu1 O6 2.0772(18) 2_544 ?
Cu1 Cu2 2.6230(5) . ?
Cu2 O2 1.9592 . ?
Cu2 O14 1.9615 4_565 ?
Cu2 O7 1.9863 4_575 ?
Cu2 O3 1.9962 . ?
Cu2 O9 2.0909(18) 3_565 ?
Cu3 O10 1.9364(18) . ?
Cu3 O5 1.9362(18) 4_676 ?
Cu3 O11 1.9522 . ?
Cu3 O12 1.9691(7) . ?
Cu3 O13 2.300(2) . ?
P4 O6 1.4967(19) . ?
P4 O5 1.5121(18) . ?
P4 C22 1.804(3) . ?
P4 C25 1.8105 . ?
P5 O9 1.4952(18) . ?
P5 O10 1.5168(18) . ?
P5 C8 1.799(3) . ?
P5 C5 1.802(3) . ?
O1 C18 1.2667 . ?
O2 C18 1.2575 . ?
O15 C14 1.243(3) . ?
O15 Cu1 1.9762 4_666 ?
O3 C1 1.251(3) . ?
O8 C31 1.261(3) . ?
O8 Cu1 1.9717 4_676 ?
O4 C1 1.229(3) . ?
O14 C14 1.251(3) . ?
O14 Cu2 1.9615 4_666 ?
C18 C19 1.500(3) . ?
C25 C30 1.390(3) . ?
C25 C26 1.410(3) . ?
O7 C31 1.234(3) . ?
O7 Cu2 1.9863 4_676 ?
C13 C8 1.389(3) . ?
C13 C12 1.403(3) . ?
C19 C24 1.392(4) . ?
C19 C20 1.401(4) . ?
C4 C3 1.392(4) . ?
C4 C5 1.392(4) . ?
C8 C9 1.402(4) . ?
C11 C12 1.396(4) . ?
C11 C10 1.402(4) . ?
C11 C14 1.500(4) . ?
C6 C5 1.395(4) . ?
C6 C7 1.396(4) . ?
C26 C27 1.372(4) . ?
C22 C23 1.396(4) . ?
C22 C21 1.401(4) . ?
C20 C21 1.384(4) . ?
C3 C2 1.387(4) . ?
C28 C29 1.391(4) . ?
C28 C27 1.401(4) . ?
C28 C31 1.499(3) . ?
C1 C2 1.515(3) . ?
C30 C29 1.386(4) . ?
C7 C2 1.399(4) . ?
C10 C9 1.384(4) . ?
C24 C23 1.386(4) . ?
O6 Cu1 2.0772(18) 2_554 ?
O9 Cu2 2.0908(18) 3_565 ?
O5 Cu3 1.9362(18) 4_575 ?
O13 C15 1.249(4) . ?
N1 C15 1.334(4) . ?
N1 C16 1.446(5) . ?
N1 C17 1.458(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Cu1 O1 88.4 . . ?
O4 Cu1 O8 170.1 . 4_575 ?
O1 Cu1 O8 88.3 . 4_575 ?
O4 Cu1 O15 90.6 . 4_565 ?
O1 Cu1 O15 167.4 . 4_565 ?
O8 Cu1 O15 90.6 4_575 4_565 ?
O4 Cu1 O6 92.18(5) . 2_544 ?
O1 Cu1 O6 98.27(6) . 2_544 ?
O8 Cu1 O6 97.55(5) 4_575 2_544 ?
O15 Cu1 O6 94.34(6) 4_565 2_544 ?
O4 Cu1 Cu2 86.75(2) . . ?
O1 Cu1 Cu2 86.99(2) . . ?
O8 Cu1 Cu2 83.74(2) 4_575 . ?
O15 Cu1 Cu2 80.40(2) 4_565 . ?
O6 Cu1 Cu2 174.62(6) 2_544 . ?
O2 Cu2 O14 168.8 . 4_565 ?
O2 Cu2 O7 90.0 . 4_575 ?
O14 Cu2 O7 87.0 4_565 4_575 ?
O2 Cu2 O3 91.4 . . ?
O14 Cu2 O3 88.7 4_565 . ?
O7 Cu2 O3 164.4 4_575 . ?
O2 Cu2 O9 93.70(6) . 3_565 ?
O14 Cu2 O9 97.28(6) 4_565 3_565 ?
O7 Cu2 O9 94.05(5) 4_575 3_565 ?
O3 Cu2 O9 101.33(5) . 3_565 ?
O2 Cu2 Cu1 81.35(2) . . ?
O14 Cu2 Cu1 87.59(2) 4_565 . ?
O7 Cu2 Cu1 83.58(2) 4_575 . ?
O3 Cu2 Cu1 81.31(2) . . ?
O9 Cu2 Cu1 174.49(5) 3_565 . ?
O10 Cu3 O5 164.13(8) . 4_676 ?
O10 Cu3 O11 85.54(6) . . ?
O5 Cu3 O11 93.95(6) 4_676 . ?
O10 Cu3 O12 93.14(6) . . ?
O5 Cu3 O12 85.71(6) 4_676 . ?
O11 Cu3 O12 173.98(5) . . ?
O10 Cu3 O13 104.41(8) . . ?
O5 Cu3 O13 91.45(8) 4_676 . ?
O11 Cu3 O13 94.34(6) . . ?
O12 Cu3 O13 91.68(6) . . ?
O6 P4 O5 116.47(11) . . ?
O6 P4 C22 110.07(11) . . ?
O5 P4 C22 108.26(11) . . ?
O6 P4 C25 110.32(8) . . ?
O5 P4 C25 107.66(8) . . ?
C22 P4 C25 103.20(9) . . ?
O9 P5 O10 116.62(11) . . ?
O9 P5 C8 109.45(11) . . ?
O10 P5 C8 106.64(11) . . ?
O9 P5 C5 110.10(11) . . ?
O10 P5 C5 106.76(11) . . ?
C8 P5 C5 106.79(12) . . ?
C18 O1 Cu1 119.1 . . ?
C18 O2 Cu2 126.3 . . ?
C14 O15 Cu1 126.86(13) . 4_666 ?
C1 O3 Cu2 124.57(12) . . ?
C31 O8 Cu1 122.22(12) . 4_676 ?
C1 O4 Cu1 120.71(12) . . ?
C14 O14 Cu2 119.01(13) . 4_666 ?
O2 C18 O1 125.1 . . ?
O2 C18 C19 116.72(10) . . ?
O1 C18 C19 118.21(10) . . ?
C30 C25 C26 119.88(16) . . ?
C30 C25 P4 120.41(12) . . ?
C26 C25 P4 119.68(12) . . ?
C31 O7 Cu2 123.13(13) . 4_676 ?
C8 C13 C12 120.25(16) . . ?
C24 C19 C20 120.0(2) . . ?
C24 C19 C18 119.4(2) . . ?
C20 C19 C18 120.6(2) . . ?
C3 C4 C5 120.1(2) . . ?
C13 C8 C9 120.2(2) . . ?
C13 C8 P5 121.25(17) . . ?
C9 C8 P5 118.4(2) . . ?
C12 C11 C10 120.0(2) . . ?
C12 C11 C14 121.0(2) . . ?
C10 C11 C14 118.9(2) . . ?
C5 C6 C7 120.3(2) . . ?
O15 C14 O14 125.5(2) . . ?
O15 C14 C11 116.2(2) . . ?
O14 C14 C11 118.3(2) . . ?
C27 C26 C25 119.7(2) . . ?
C23 C22 C21 119.6(2) . . ?
C23 C22 P4 119.2(2) . . ?
C21 C22 P4 121.0(2) . . ?
C21 C20 C19 119.7(2) . . ?
C2 C3 C4 119.9(2) . . ?
C4 C5 C6 119.8(2) . . ?
C4 C5 P5 119.4(2) . . ?
C6 C5 P5 120.74(19) . . ?
C29 C28 C27 119.5(2) . . ?
C29 C28 C31 119.7(2) . . ?
C27 C28 C31 120.5(2) . . ?
C20 C21 C22 120.4(2) . . ?
O4 C1 O3 126.3(2) . . ?
O4 C1 C2 118.6(2) . . ?
O3 C1 C2 115.1(2) . . ?
O7 C31 O8 124.8(2) . . ?
O7 C31 C28 119.2(2) . . ?
O8 C31 C28 115.8(2) . . ?
C29 C30 C25 119.9(2) . . ?
C2 C7 C6 119.2(2) . . ?
C30 C29 C28 120.3(2) . . ?
C9 C10 C11 120.5(2) . . ?
C23 C24 C19 120.3(3) . . ?
C10 C9 C8 119.6(2) . . ?
C3 C2 C7 120.5(2) . . ?
C3 C2 C1 120.0(2) . . ?
C7 C2 C1 119.4(2) . . ?
C26 C27 C28 120.5(2) . . ?
C11 C12 C13 119.4(2) . . ?
C24 C23 C22 120.1(3) . . ?
P4 O6 Cu1 166.66(12) . 2_554 ?
P5 O9 Cu2 161.57(12) . 3_565 ?
P4 O5 Cu3 129.96(12) . 4_575 ?
P5 O10 Cu3 127.98(11) . . ?
C15 O13 Cu3 119.2(2) . . ?
C15 N1 C16 121.7(3) . . ?
C15 N1 C17 120.7(3) . . ?
C16 N1 C17 117.6(3) . . ?
O13 C15 N1 124.8(3) . . ?

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        76.63
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         1.021
_refine_diff_density_min         -0.775
_refine_diff_density_rms         0.099

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.026 0.001 1.000 959 342 ' '
2 -0.204 0.499 0.500 959 343 ' '
_platon_squeeze_details          
;
;
####################################################################### 
# 
# 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_c:FJI-C5
_database_code_depnum_ccdc_archive 'CCDC 1444653'
_audit_update_record             
;
2015-12-28 deposited with the CCDC.
2018-03-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H16 Mg3 N0 O16 P2'
_chemical_formula_weight         743.28

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mg Mg 0.1719 0.1771 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P n n m'

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

_cell_length_a                   11.3020(2)
_cell_length_b                   13.5426(2)
_cell_length_c                   15.7763(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2414.70(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    6206
_cell_measurement_theta_min      4.2900
_cell_measurement_theta_max      72.6000

_exptl_crystal_description       rodlike
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.022
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             756
_exptl_absorpt_coefficient_mu    1.655
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8520
_exptl_absorpt_correction_T_max  0.9520
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger.

The calculated free volume of FJI-C5 with removal of guest solvent molecules is 44.2% by PLATON (1.8 Angstrom probe radius). We employed 
PLATON SQUEEZE to calculate the contribution to the contribution to the diffraction 
from the solvent region and thereby produced a set of solvent-free diffraction intensities. 
The final formula was calculated from TGA and elemental analysis data. 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.5594
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15692
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_sigmaI/netI    0.0260
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         4.30
_diffrn_reflns_theta_max         72.69
_reflns_number_total             2478
_reflns_number_gt                2170
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1030P)²+6.2019P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2478
_refine_ls_number_parameters     116
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0827
_refine_ls_R_factor_gt           0.0765
_refine_ls_wR_factor_ref         0.2102
_refine_ls_wR_factor_gt          0.2051
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_restrained_S_all      1.220
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.5000 0.5000 0.14063(7) 0.0240(4) Uani 1 2 d S . .
Mg1 Mg 0.5000 0.0000 0.5000 0.0159(5) Uani 1 4 d S . .
Mg2 Mg 0.80424(14) 0.08963(11) 0.5000 0.0219(4) Uani 1 2 d SU . .
O1 O 0.5198(2) 0.1057(2) 0.40741(17) 0.0297(6) Uani 1 1 d . . .
O4 O 0.8881(3) 0.0192(2) 0.59311(16) 0.0373(8) Uani 1 1 d . . .
O5 O 0.9268(4) 0.2056(3) 0.5000 0.0538(14) Uani 1 2 d S . .
C5 C 0.5284(3) 0.3974(3) 0.2116(2) 0.0217(7) Uani 1 1 d . . .
C2 C 0.5748(3) 0.2438(3) 0.3249(2) 0.0256(8) Uani 1 1 d . . .
C1 C 0.6011(3) 0.1611(3) 0.3865(3) 0.0287(8) Uani 1 1 d U . .
C3 C 0.4643(4) 0.2535(4) 0.2873(3) 0.0375(10) Uani 1 1 d . . .
H3 H 0.4035 0.2075 0.3001 0.045 Uiso 1 1 calc R . .
O2 O 0.7030(3) 0.1574(3) 0.4128(3) 0.0869(15) Uani 1 1 d U . .
C4 C 0.4424(4) 0.3305(4) 0.2306(3) 0.0374(10) Uani 1 1 d . . .
H4 H 0.3666 0.3364 0.2050 0.045 Uiso 1 1 calc R . .
C6 C 0.6389(4) 0.3885(3) 0.2492(3) 0.0375(10) Uani 1 1 d . . .
H6 H 0.6997 0.4344 0.2357 0.045 Uiso 1 1 calc R . .
C7 C 0.6611(2) 0.3132(2) 0.3061(3) 0.0442(12) Uani 1 1 d . . .
H7 H 0.7364 0.3090 0.3327 0.053 Uiso 1 1 calc R . .
O3 O 0.6835(2) -0.0388(2) 0.5000(3) 0.0254(8) Uani 1 2 d SR . .


_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
P1 O4 1.493(3) 7_765 ?
P1 O4 1.493(3) 8_565 ?
P1 C5 1.812(3) 2_665 ?
P1 C5 1.812(3) . ?
Mg1 O1 2.058(2) 6_556 ?
Mg1 O1 2.058(2) 5_656 ?
Mg1 O1 2.058(2) . ?
Mg1 O1 2.058(2) 2_655 ?
Mg1 O3 2.140(3) . ?
Mg1 O3 2.140(3) 5_656 ?
Mg1 Mg2 3.6465(16) 5_656 ?
Mg1 Mg2 3.6465(16) . ?
Mg2 O4 1.992(3) 6_556 ?
Mg2 O4 1.992(3) . ?
Mg2 O2 2.011(4) . ?
Mg2 O2 2.011(4) 6_556 ?
Mg2 O5 2.094(4) . ?
Mg2 O3 2.211(3) . ?
O1 C1 1.231(4) . ?
O4 P1 1.493(3) 7_756 ?
C5 C4 1.362(6) . ?
C5 C6 1.389(5) . ?
C2 C7 1.387(5) . ?
C2 C3 1.388(5) . ?
C2 C1 1.513(5) . ?
C1 O2 1.225(5) . ?
C3 C4 1.397(6) . ?
C6 C7 1.381(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 P1 O4 119.7(3) 7_765 8_565 ?
O4 P1 C5 109.08(17) 7_765 2_665 ?
O4 P1 C5 107.06(15) 8_565 2_665 ?
O4 P1 C5 107.06(15) 7_765 . ?
O4 P1 C5 109.08(17) 8_565 . ?
C5 P1 C5 103.7(2) 2_665 . ?
O1 Mg1 O1 89.55(16) 6_556 5_656 ?
O1 Mg1 O1 90.45(16) 6_556 . ?
O1 Mg1 O1 180.0 5_656 . ?
O1 Mg1 O1 179.998(1) 6_556 2_655 ?
O1 Mg1 O1 90.45(16) 5_656 2_655 ?
O1 Mg1 O1 89.55(16) . 2_655 ?
O1 Mg1 O3 93.77(14) 6_556 . ?
O1 Mg1 O3 86.23(12) 5_656 . ?
O1 Mg1 O3 93.77(12) . . ?
O1 Mg1 O3 86.23(14) 2_655 . ?
O1 Mg1 O3 86.23(14) 6_556 5_656 ?
O1 Mg1 O3 93.77(12) 5_656 5_656 ?
O1 Mg1 O3 86.23(12) . 5_656 ?
O1 Mg1 O3 93.76(14) 2_655 5_656 ?
O3 Mg1 O3 180.0 . 5_656 ?
O1 Mg1 Mg2 109.51(7) 6_556 5_656 ?
O1 Mg1 Mg2 70.49(7) 5_656 5_656 ?
O1 Mg1 Mg2 109.51(7) . 5_656 ?
O1 Mg1 Mg2 70.49(7) 2_655 5_656 ?
O3 Mg1 Mg2 146.33(8) . 5_656 ?
O3 Mg1 Mg2 33.66(8) 5_656 5_656 ?
O1 Mg1 Mg2 70.49(7) 6_556 . ?
O1 Mg1 Mg2 109.51(7) 5_656 . ?
O1 Mg1 Mg2 70.49(7) . . ?
O1 Mg1 Mg2 109.51(7) 2_655 . ?
O3 Mg1 Mg2 33.67(8) . . ?
O3 Mg1 Mg2 146.33(8) 5_656 . ?
Mg2 Mg1 Mg2 180.0 5_656 . ?
O4 Mg2 O4 95.0(2) 6_556 . ?
O4 Mg2 O2 89.1(2) 6_556 . ?
O4 Mg2 O2 173.71(17) . . ?
O4 Mg2 O2 173.71(17) 6_556 6_556 ?
O4 Mg2 O2 89.1(2) . 6_556 ?
O2 Mg2 O2 86.4(3) . 6_556 ?
O4 Mg2 O5 92.55(12) 6_556 . ?
O4 Mg2 O5 92.55(12) . . ?
O2 Mg2 O5 91.98(15) . . ?
O2 Mg2 O5 91.98(15) 6_556 . ?
O4 Mg2 O3 85.21(14) 6_556 . ?
O4 Mg2 O3 85.21(13) . . ?
O2 Mg2 O3 90.44(16) . . ?
O2 Mg2 O3 90.44(17) 6_556 . ?
O5 Mg2 O3 176.68(16) . . ?
O4 Mg2 Mg1 106.81(10) 6_556 . ?
O4 Mg2 Mg1 106.81(10) . . ?
O2 Mg2 Mg1 67.37(11) . . ?
O2 Mg2 Mg1 67.37(11) 6_556 . ?
O5 Mg2 Mg1 150.87(14) . . ?
O3 Mg2 Mg1 32.45(7) . . ?
C1 O1 Mg1 134.0(2) . . ?
P1 O4 Mg2 148.95(19) 7_756 . ?
C4 C5 C6 119.3(3) . . ?
C4 C5 P1 121.3(3) . . ?
C6 C5 P1 119.4(3) . . ?
C7 C2 C3 118.5(3) . . ?
C7 C2 C1 120.1(3) . . ?
C3 C2 C1 121.4(3) . . ?
O2 C1 O1 125.9(3) . . ?
O2 C1 C2 115.6(3) . . ?
O1 C1 C2 118.4(3) . . ?
C2 C3 C4 120.2(4) . . ?
C1 O2 Mg2 141.7(3) . . ?
C5 C4 C3 120.8(4) . . ?
C7 C6 C5 120.4(4) . . ?
C6 C7 C2 120.8(3) . . ?
Mg1 O3 Mg2 113.88(13) . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        72.69
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         1.289
_refine_diff_density_min         -1.323
_refine_diff_density_rms         0.093

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.018 0.000 0.000 533 155 ' '
2 -0.008 0.500 0.500 533 155 ' '
_platon_squeeze_details          
;
;
