# Electronic Supplementary Material (ESI) for Chemical Communications.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1976143'
loop_
_audit_author_name
_audit_author_address
EDC-PF
;Northwest University
China
;
_audit_update_record             
;
2020-01-08 deposited with the CCDC.	2020-02-10 downloaded from the CCDC.
;


#=====================================================================
# start Validation Reply Form


_vrf_PLAT933_1                   
;
RESPONSE: 
These reflections were omitted due to the affection by
beamstop.
;


_vrf_PLAT051_1                   
;
RESPONSE: 
In each unit cell, 20 severely disordered acetonitrile molecules
were removed by PLATON's SQUEEZE subroutine so they are included in
cif reported Mu value but are not included in the calculated Mu 
value which is only based on the structure model. 
;

_vrf_FORMU01_1                   
;
RESPONSE: 
In each unit cell, 20 severely disordered acetonitrile molecules
were removed by PLATON's SQUEEZE subroutine so they does not include in
the structure model and _atom_site_* section of cif file. But the reported
formula includes the solvents, which causes the atom counts discrepancy.
;


_vrf_CELLZ01_1                   
;
RESPONSE: 
In each unit cell, 20 severely disordered acetonitrile molecules
were removed by PLATON's SQUEEZE subroutine so they does not include in
the structure model and _atom_site_* section of cif file. But the reported
formula includes the solvents, which causes the formula discrepancy
between the one calculated from atom_site data and the reported one.
;

_vrf_PLAT041_1                   
;
RESPONSE: 
In each unit cell, 20 severely disordered acetonitrile molecules
were removed by PLATON's SQUEEZE subroutine so they does not include in
the structure model and _atom_site_* section of cif file. But the reported
formula includes the solvents, which causes the discrepancy between the
calculated SumFormula and the reported SumFormula.
;

_vrf_PLAT042_1                   
;
RESPONSE: 
In each unit cell, 20 severely disordered acetonitrile molecules
were removed by PLATON's SQUEEZE subroutine so they does not include in
the structure model and calculated MoietyFormula of cif file. But the reported
MoietyFormula includes the solvents, which causes the discrepancy between the
calculated and the reported MoietyFormula.
;

_vrf_PLAT068_1                   
;
RESPONSE: 
In each unit cell, 20 severely disordered acetonitrile molecules
were removed by PLATON's SQUEEZE subroutine so they does not include in
the structure model and _atom_site_* section of cif file. The reported F000
counts these two n-hexane molecules while the calculated F000 does not,
which causes the discrepancy between these two.
;



_vrf_PLAT606_1                   
;
RESPONSE: 
SQUEEZE was applied to remove 20 severely disordered 
acetonitrile moleculesin the unit cell, thus leaving large voids.
;

_vrf_PLAT868_1                   
;
RESPONSE: 
In each unit cell, there are 20 severely disordered acetonitrile molecules 
that were hard to modeled by disorders. So they were removed by using masks.
;

# end Validation Reply Form 
#=====================================================================



_audit_creation_date             2019-09-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C126 H172 N4 O8 P8 Pt4, 4(C F3 O3 S), 17(C3 H6 O)'
_chemical_formula_sum            'C90 H82 F24 N18 P4'
_chemical_formula_weight         1995.61
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0137 0.0070 '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'
F F 0.0583 0.0400 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0241 0.0136 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2543 0.3332 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           94
_space_group_name_H-M_alt        'P 42 21 2'
_space_group_name_Hall           'P 4n 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y, x, -z'
'-y, -x, -z'

_cell_length_a                   19.429(4)
_cell_length_b                   19.429(4)
_cell_length_c                   12.057(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4551(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9830
_cell_measurement_theta_min      2.98
_cell_measurement_theta_max      55.02
_cell_measurement_temperature    180(2)
_shelx_estimated_absorpt_T_max   0.908
_shelx_estimated_absorpt_T_min   0.836
_exptl_absorpt_coefficient_mu    1.096
_exptl_absorpt_correction_T_min  0.8753
_exptl_absorpt_correction_T_max  0.9562
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used 
for absorption correction.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0772
_diffrn_reflns_av_unetI/netI     0.0486
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            30148
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.917
_diffrn_reflns_theta_min         3.959
_diffrn_ambient_temperature      180.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON 100 CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34138
_diffrn_source                   'Liquid METALJET D2 PLUS X-ray Source'
_reflns_Friedel_coverage         0.734
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                3598
_reflns_number_total             4325
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (bruker, 2016)'
_computing_data_collection       'APEX3 v.2017.3-0 (Bruker AXS Inc., 2017)'
_computing_data_reduction        'SAINT V8.38A (bruker, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'


_refine_diff_density_max         0.241
_refine_diff_density_min         -0.219
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details 
;
 Flack x determined using 1313 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.019(12)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         4325
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0454
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0868P)²+0.6448P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1378
_refine_ls_wR_factor_ref         0.1420
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C9(H9), C10(H10), C11(H11), C13(H13),
 C14(H14), C17(H17), C18(H18)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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
P1 P 0.60864(5) 0.82949(6) 0.10402(9) 0.0524(3) Uani 1 1 d . . . . .
F1 F 0.64757(18) 0.77670(19) 0.1830(3) 0.0884(10) Uani 1 1 d . . . . .
F2 F 0.67149(17) 0.8296(2) 0.0221(2) 0.0959(10) Uani 1 1 d . . . . .
F3 F 0.56805(18) 0.88155(19) 0.0265(3) 0.1048(13) Uani 1 1 d . . . . .
F4 F 0.54642(16) 0.8295(2) 0.1902(3) 0.0982(11) Uani 1 1 d . . . . .
F5 F 0.57267(18) 0.76884(17) 0.0403(3) 0.0865(9) Uani 1 1 d . . . . .
F6 F 0.64335(15) 0.89236(17) 0.1688(3) 0.0767(8) Uani 1 1 d . . . . .
N1 N 0.64236(15) 0.87951(14) 0.4359(2) 0.0402(7) Uani 1 1 d . . . . .
N2 N 0.56316(15) 0.80183(15) 0.4498(2) 0.0396(6) Uani 1 1 d . . . . .
C1 C 0.8295(2) 0.7960(2) 0.7345(3) 0.0504(9) Uani 1 1 d . . . . .
H1 H 0.860732 0.762979 0.763413 0.060 Uiso 1 1 calc R . . . .
C2 C 0.7902(3) 0.8332(3) 0.8049(3) 0.0589(12) Uani 1 1 d . . . . .
H2 H 0.795117 0.826786 0.882626 0.071 Uiso 1 1 calc R . . . .
C3 C 0.7418(3) 0.8819(2) 0.7645(3) 0.0575(10) Uani 1 1 d . . . . .
H3 H 0.714211 0.907369 0.814929 0.069 Uiso 1 1 calc R . . . .
C4 C 0.7350(2) 0.8918(2) 0.6540(3) 0.0507(9) Uani 1 1 d . . . . .
H4 H 0.702108 0.924192 0.628183 0.061 Uiso 1 1 calc R . . . .
C5 C 0.77547(19) 0.85525(18) 0.5752(3) 0.0397(7) Uani 1 1 d . . . . .
C6 C 0.76685(19) 0.86403(18) 0.4601(3) 0.0406(7) Uani 1 1 d . . . . .
C7 C 0.80572(18) 0.82466(18) 0.3836(3) 0.0397(7) Uani 1 1 d . . . . .
C8 C 0.71179(19) 0.91140(18) 0.4202(3) 0.0444(8) Uani 1 1 d . . . . .
H8A H 0.719050 0.921611 0.340571 0.053 Uiso 1 1 calc R . . . .
H8B H 0.714180 0.955300 0.461671 0.053 Uiso 1 1 calc R . . . .
C9 C 0.5810(2) 0.9135(2) 0.4565(4) 0.0546(10) Uani 1 1 d . . . . .
H9 H 0.574850 0.961832 0.462370 0.065 Uiso 1 1 calc R . . . .
C10 C 0.5309(2) 0.8641(2) 0.4669(4) 0.0517(9) Uani 1 1 d . . . . .
H10 H 0.483525 0.871444 0.482596 0.062 Uiso 1 1 calc R . . . .
C11 C 0.63012(19) 0.81219(18) 0.4320(3) 0.0418(8) Uani 1 1 d . . . . .
H11 H 0.663450 0.777373 0.418744 0.050 Uiso 1 1 calc R . . . .
C12 C 0.53378(17) 0.73412(16) 0.4574(3) 0.0363(7) Uani 1 1 d . . . . .
C13 C 0.55649(19) 0.68552(18) 0.3822(3) 0.0399(7) Uani 1 1 d . . . . .
H13 H 0.585552 0.698120 0.322205 0.048 Uiso 1 1 calc R . . . .
C14 C 0.53552(19) 0.61711(19) 0.3969(3) 0.0414(7) Uani 1 1 d . . . . .
H14 H 0.550929 0.582842 0.346509 0.050 Uiso 1 1 calc R . . . .
C15 C 0.49240(17) 0.59856(17) 0.4844(3) 0.0383(7) Uani 1 1 d . . . . .
C16 C 0.47553(18) 0.52447(18) 0.500000 0.0382(10) Uani 1 2 d S T P . .
C17 C 0.46695(18) 0.64971(19) 0.5531(3) 0.0435(8) Uani 1 1 d . . . . .
H17 H 0.434095 0.638131 0.608438 0.052 Uiso 1 1 calc R . . . .
C18 C 0.48848(18) 0.71755(19) 0.5429(3) 0.0422(8) Uani 1 1 d . . . . .
H18 H 0.472712 0.751841 0.592984 0.051 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
P1 F1 1.591(3) . ?
P1 F2 1.571(3) . ?
P1 F3 1.587(3) . ?
P1 F4 1.594(3) . ?
P1 F5 1.571(3) . ?
P1 F6 1.599(3) . ?
N1 C8 1.497(4) . ?
N1 C9 1.384(5) . ?
N1 C11 1.330(4) . ?
N2 C10 1.379(5) . ?
N2 C11 1.334(5) . ?
N2 C12 1.437(4) . ?
C1 C2 1.351(6) . ?
C1 C7 1.440(5) 7_556 ?
C2 C3 1.420(7) . ?
C3 C4 1.352(6) . ?
C4 C5 1.423(5) . ?
C5 C6 1.408(5) . ?
C5 C7 1.445(5) 7_556 ?
C6 C7 1.417(5) . ?
C6 C8 1.491(5) . ?
C9 C10 1.373(5) . ?
C12 C13 1.381(5) . ?
C12 C18 1.394(5) . ?
C13 C14 1.401(5) . ?
C14 C15 1.394(5) . ?
C15 C16 1.488(4) . ?
C15 C17 1.385(5) . ?
C16 C16 1.344(10) 2_665 ?
C17 C18 1.388(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
F1 P1 F4 88.3(2) . . ?
F1 P1 F6 89.95(18) . . ?
F2 P1 F1 90.46(19) . . ?
F2 P1 F3 90.9(2) . . ?
F2 P1 F4 178.29(19) . . ?
F2 P1 F5 92.3(2) . . ?
F2 P1 F6 88.76(18) . . ?
F3 P1 F1 178.6(2) . . ?
F3 P1 F4 90.4(2) . . ?
F3 P1 F6 90.60(18) . . ?
F4 P1 F6 90.07(19) . . ?
F5 P1 F1 91.2(2) . . ?
F5 P1 F3 88.22(19) . . ?
F5 P1 F4 88.9(2) . . ?
F5 P1 F6 178.46(19) . . ?
C9 N1 C8 127.0(3) . . ?
C11 N1 C8 124.3(3) . . ?
C11 N1 C9 108.7(3) . . ?
C10 N2 C12 127.9(3) . . ?
C11 N2 C10 109.6(3) . . ?
C11 N2 C12 122.4(3) . . ?
C2 C1 C7 121.0(4) . 7_556 ?
C1 C2 C3 121.0(4) . . ?
C4 C3 C2 119.8(4) . . ?
C3 C4 C5 122.2(4) . . ?
C4 C5 C7 117.9(3) . 7_556 ?
C6 C5 C4 122.2(4) . . ?
C6 C5 C7 119.9(3) . 7_556 ?
C5 C6 C7 120.9(3) . . ?
C5 C6 C8 118.6(3) . . ?
C7 C6 C8 120.3(3) . . ?
C1 C7 C5 118.1(3) 7_556 7_556 ?
C6 C7 C1 122.7(4) . 7_556 ?
C6 C7 C5 119.2(3) . 7_556 ?
C6 C8 N1 110.5(3) . . ?
C10 C9 N1 107.1(3) . . ?
C9 C10 N2 106.0(3) . . ?
N1 C11 N2 108.5(3) . . ?
C13 C12 N2 117.2(3) . . ?
C13 C12 C18 122.0(3) . . ?
C18 C12 N2 120.6(3) . . ?
C12 C13 C14 118.2(3) . . ?
C15 C14 C13 121.0(3) . . ?
C14 C15 C16 118.6(3) . . ?
C17 C15 C14 118.8(3) . . ?
C17 C15 C16 122.6(3) . . ?
C15 C16 C15 116.2(4) 8_666 . ?
C16 C16 C15 121.9(2) 2_665 8_666 ?
C16 C16 C15 121.9(2) 2_665 . ?
C15 C17 C18 121.3(3) . . ?
C17 C18 C12 118.4(3) . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.082 0.346 0.500 815.9 216.4 10(C2H3N)
2 -0.536 -0.373 0.000 815.9 216.1 10(C2H3N)

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1_a
_database_code_depnum_ccdc_archive 'CCDC 1976144'
loop_
_audit_author_name
_audit_author_address
DC-Cl
;Northwest University
China
;
_audit_update_record             
;
2020-01-08 deposited with the CCDC.	2020-02-10 downloaded from the CCDC.
;

#=====================================================================
# start Validation Reply Form

_vrf_PLAT340_1_a                 
;
RESPONSE: 
Single crystals of this complex from 
different batches of crystal growth were measured. 
However, no crystals provided structural data set 
better than the reported one. All measurements were 
performed at low temperature (100K) but none of 
them was able to yield diffractions to high 
resolution with strong enough reflection intensity 
due to the severe disorders of solvent molecules. 
The low resolution data causes high Rint value and the low bond 
precision. In terms of the reported data, all 
available geometric data up to the given 
2theta-limit were collected with an optimized 
data collection strategy, to insure that no 
reflection could be missed due to improper data 
collection strategy. Reported data set of this 
complex has a completeness of 0.995 (very close to 1), 
indicating the data set's quality is not poor.
;


_vrf_PLAT906_1_a                 
;
RESPONSE: 
The K value is large only for weak reflections with
Fc/Fcmax lower than 0.021.
;

_vrf_FORMU01_1_a                 
;
RESPONSE: 
In each unit cell, 3 severely disordered methanol molecules
were removed by PLATON's SQUEEZE subroutine so it does not include in
the structure model and _atom_site_* section of cif file. But the reported
formula includes the solvents, which causes the atom counts discrepancy.
;


_vrf_CELLZ01_1_a                 
;
RESPONSE: 
In each unit cell, 3 severely disordered methanol molecules
were removed by PLATON's SQUEEZE subroutine so it does not include in
the structure model and _atom_site_* section of cif file. But the reported
formula includes the solvents, which causes the formula discrepancy
between the one calculated from atom_site data and the reported one.
;

_vrf_PLAT041_1_a                 
;
RESPONSE: 
In each unit cell, 3 severely disordered methanol molecules
were removed by PLATON's SQUEEZE subroutine so it does not include in
the structure model and _atom_site_* section of cif file. But the reported
formula includes the solvents, which causes the discrepancy between the
calculated SumFormula and the reported SumFormula.
;

_vrf_PLAT068_1_a                 
;
RESPONSE: 
In each unit cell, 3 severely disordered methanol molecules
were removed by PLATON's SQUEEZE subroutine so it does not include in
the structure model and _atom_site_* section of cif file. The reported F000
counts these two n-hexane molecules while the calculated F000 does not,
which causes the discrepancy between these two.
;

_vrf_PLAT260_1_a                 
;
RESPONSE: 
The methanol solvent molecules are highly disordered so their 
atoms' atomic displacement parameters are higher than 
other atoms. 
;

_vrf_PLAT051_1_a                 
;
RESPONSE: 
In each unit cell, 3 severely disordered methanol molecules
were removed by PLATON's SQUEEZE subroutine so it does not include in
the structure model and the calculation of Mu(calc). The reported Mu 
value in cif file, however, put these removed solvent molecules into 
consideration, which cuases the Mu(CIF) is different from Mu(calc). 
;


_vrf_PLAT042_1_a                 
;
RESPONSE: 
In each unit cell, 3 severely disordered methanol molecules
were removed by PLATON's SQUEEZE subroutine so it does not include in
the calculated MoietyFormula, which is only based on structure model.
;

_vrf_PLAT606_1_a                 
;
RESPONSE: 
SQUEEZE was applied to remove 3 severely disordered methanol molecules 
in the unit cell, thus leaving large voids.
;

_vrf_PLAT868_1_a                 
;
RESPONSE: 
In each unit cell, 3 severely disordered methanol molecules that 
can not de modeled by disorders, so SQUEEZE was applied to remove them.
;


# end Validation Reply Form 
#=====================================================================

_audit_creation_date             2019-09-13
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C54 H44 N8, 7.5(C H4 O), 4(Cl)'
_chemical_formula_sum            'C61.50 H74 Cl4 N8 O7.50'
_chemical_formula_weight         1187.08
_chemical_melting_point          ?
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.8059(14)
_cell_length_b                   14.764(2)
_cell_length_c                   19.268(2)
_cell_angle_alpha                78.553(5)
_cell_angle_beta                 73.274(4)
_cell_angle_gamma                75.000(5)
_cell_volume                     3078.7(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9439
_cell_measurement_temperature    114(2)
_cell_measurement_theta_min      2.96
_cell_measurement_theta_max      26.38
_shelx_estimated_absorpt_T_max   0.985
_shelx_estimated_absorpt_T_min   0.970
_exptl_absorpt_coefficient_mu    0.251
_exptl_absorpt_correction_T_min  0.5720
_exptl_absorpt_correction_T_max  0.6307
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for 
absorption correction. The 
Ratio of minimum to maximum transmission is 
0.9069. The λ/2 correction factor is Not present.
;
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1254
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0570
_diffrn_reflns_av_unetI/netI     0.0590
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            49040
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.056
_diffrn_reflns_theta_max         25.056
_diffrn_reflns_theta_min         2.228
_diffrn_ambient_temperature      114(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON 100 CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7281
_reflns_number_total             10847
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_data_collection       'APEX3 v.2017.3-0 (Bruker AXS Inc., 2017)'
_computing_cell_refinement       'SAINT V8.38A (bruker, 2016)'
_computing_data_reduction        'SAINT V8.38A (bruker, 2016)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Xshell v.6.3.1 (Bruker AXS Inc., 2016)'
_computing_publication_material  'APEX3 v.2017.3-0 (Bruker AXS Inc., 2017)'
_refine_diff_density_max         1.050
_refine_diff_density_min         -0.806
_refine_diff_density_rms         0.067
_refine_ls_extinction_coef       0.0043(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     757
_refine_ls_number_reflns         10847
_refine_ls_number_restraints     88
_refine_ls_R_factor_all          0.1066
_refine_ls_R_factor_gt           0.0725
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0983P)²+2.6213P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1814
_refine_ls_wR_factor_ref         0.2024
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O3-C56
 1.406 with sigma of 0.005
 O3X-C56X
 1.406 with sigma of 0.005
 O1-C54 = O1X-C54X
 1.406 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
O3 \\sim C56: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
O3 \\sim C56 \\sim O3X \\sim C56X: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
O1 \\sim C54 \\sim O1X \\sim C54X: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 O3, C56
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O3, C56, O3X, C56X
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1, C54, O1X, C54X
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O3X)=Sof(H3X)=Sof(C56X)=Sof(H56D)=Sof(H56E)=Sof(H56F)=Sof(O1X)=Sof(H1X)=
 Sof(C54X)=Sof(H54D)=Sof(H54E)=Sof(H54F)=1-FVAR(1)
 Sof(O1)=Sof(H1)=Sof(C54)=Sof(H54A)=Sof(H54B)=Sof(H54C)=Sof(O3)=Sof(H3A)=
 Sof(C56)=Sof(H56A)=Sof(H56B)=Sof(H56C)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C18(H18A,H18B), C38(H38A,H38B), C45(H45A,H45B)
6.b Aromatic/amide H refined with riding coordinates:
 C0AA(H0AA), C3(H3), C4(H4), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10),
 C13(H13), C14(H14), C16(H16), C17(H17), C19(H19), C20(H20), C21(H21), C23(H23),
  C24(H24), C26(H26), C27(H27), C30(H30), C31(H31), C33(H33), C34(H34),
 C35(H35), C36(H36), C37(H37), C40(H40), C41(H41), C43(H43), C44(H44), C46(H46),
  C47(H47), C48(H48), C50(H50), C51(H51), C53(H53)
6.c Idealised Me refined as rotating group:
 C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C57(H57A,H57B,
 H57C), C59(H59A,H59B,H59C), C021(H02A,H02B,H02C), C56X(H56D,H56E,H56F),
 C54X(H54D,H54E,H54F)
6.d Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2), O3(H3A), O6(H6A), O5(H5), O4(H4A), O3X(H3X), O1X(H1X)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl1 Cl 0.43666(10) 0.21343(7) 0.16555(6) 0.0497(3) Uani 1 1 d . . . . .
Cl2 Cl -0.38307(9) 0.22073(7) 0.46049(6) 0.0430(3) Uani 1 1 d . . . . .
Cl3 Cl 0.23510(15) 0.32981(11) 0.89072(9) 0.0840(5) Uani 1 1 d . . . . .
Cl4 Cl 0.94176(10) 0.27576(7) 0.70950(7) 0.0559(3) Uani 1 1 d . . . . .
O1 O 0.7008(6) 0.0981(4) 0.1182(4) 0.0678(19) Uani 0.633(7) 1 d D U P A 1
H1 H 0.632330 0.134849 0.123059 0.102 Uiso 0.633(7) 1 calc GR . P A 1
C54 C 0.7910(7) 0.1512(6) 0.0936(6) 0.064(2) Uani 0.633(7) 1 d D U P A 1
H54A H 0.770880 0.201611 0.054717 0.096 Uiso 0.633(7) 1 calc GR . P A 1
H54B H 0.869098 0.109865 0.074497 0.096 Uiso 0.633(7) 1 calc GR . P A 1
H54C H 0.796108 0.179268 0.134318 0.096 Uiso 0.633(7) 1 calc GR . P A 1
O2 O -0.1109(2) 0.22490(19) 0.41602(17) 0.0444(7) Uani 1 1 d . . . . .
H2 H -0.185349 0.230890 0.420752 0.067 Uiso 1 1 calc GR . . . .
C55 C -0.0860(4) 0.3140(3) 0.4124(3) 0.0721(17) Uani 1 1 d . . . . .
H55A H -0.105253 0.354838 0.368822 0.108 Uiso 1 1 calc GR . . . .
H55B H 0.000016 0.306507 0.409848 0.108 Uiso 1 1 calc GR . . . .
H55C H -0.135307 0.342643 0.456191 0.108 Uiso 1 1 calc GR . . . .
O3 O 0.5098(6) 0.1481(5) 0.3491(4) 0.090(2) Uani 0.633(7) 1 d D U P A 1
H3A H 0.534073 0.154646 0.384357 0.135 Uiso 0.633(7) 1 calc GR . P A 1
C56 C 0.5877(13) 0.0712(12) 0.3150(12) 0.110(5) Uani 0.633(7) 1 d D U P A 1
H56A H 0.659684 0.091444 0.281914 0.165 Uiso 0.633(7) 1 calc GR . P A 1
H56B H 0.545693 0.048608 0.286980 0.165 Uiso 0.633(7) 1 calc GR . P A 1
H56C H 0.612245 0.020060 0.352205 0.165 Uiso 0.633(7) 1 calc GR . P A 1
O6 O 0.6699(3) 0.3237(3) 0.7132(2) 0.0782(11) Uani 1 1 d . . . . .
H6A H 0.739117 0.321941 0.717787 0.117 Uiso 1 1 calc GR . . . .
C57 C 0.6470(6) 0.3897(4) 0.6552(4) 0.098(2) Uani 1 1 d . . . . .
H57A H 0.710213 0.374352 0.610814 0.147 Uiso 1 1 calc GR . . . .
H57B H 0.646542 0.452536 0.664903 0.147 Uiso 1 1 calc GR . . . .
H57C H 0.568029 0.389568 0.648284 0.147 Uiso 1 1 calc GR . . . .
O5 O 0.8845(3) 0.1316(3) 0.8505(2) 0.0790(11) Uani 1 1 d . . . . .
H5 H 0.898510 0.151381 0.805498 0.118 Uiso 1 1 calc GR . . . .
C59 C 0.9957(6) 0.0889(5) 0.8699(3) 0.096(2) Uani 1 1 d . . . . .
H59A H 1.034764 0.138232 0.873453 0.143 Uiso 1 1 calc GR . . . .
H59B H 1.049174 0.050200 0.832375 0.143 Uiso 1 1 calc GR . . . .
H59C H 0.979970 0.048712 0.917115 0.143 Uiso 1 1 calc GR . . . .
O4 O 0.2907(3) 0.1397(2) 0.98722(18) 0.0554(8) Uani 1 1 d . . . . .
H4A H 0.280895 0.194133 0.963484 0.083 Uiso 1 1 calc GR . . . .
C021 C 0.1952(5) 0.0974(4) 0.9892(3) 0.0630(13) Uani 1 1 d . . . . .
H02A H 0.117509 0.139002 1.008617 0.095 Uiso 1 1 calc GR . . . .
H02B H 0.202328 0.036413 1.020802 0.095 Uiso 1 1 calc GR . . . .
H02C H 0.199445 0.087395 0.939682 0.095 Uiso 1 1 calc GR . . . .
N1 N 0.1592(3) 0.4211(2) 0.27246(17) 0.0309(7) Uani 1 1 d . . . . .
N2 N 0.1219(3) 0.3843(2) 0.17912(17) 0.0352(7) Uani 1 1 d . . . . .
N3 N 0.0696(3) -0.0314(2) 0.35633(17) 0.0310(7) Uani 1 1 d . . . . .
N4 N 0.1539(2) -0.00104(19) 0.43260(16) 0.0284(7) Uani 1 1 d . . . . .
N5 N 0.4906(3) 0.1152(2) 0.82345(16) 0.0310(7) Uani 1 1 d . . . . .
N6 N 0.5704(3) 0.1304(2) 0.90730(16) 0.0321(7) Uani 1 1 d . . . . .
N7 N 0.3975(3) 0.5898(2) 0.82144(17) 0.0358(8) Uani 1 1 d . . . . .
N8 N 0.3457(3) 0.5654(2) 0.72878(17) 0.0302(7) Uani 1 1 d . . . . .
C0AA C 0.2329(3) 0.4579(2) 0.7124(2) 0.0296(8) Uani 1 1 d . . . . .
H0AA H 0.191771 0.455166 0.762747 0.035 Uiso 1 1 calc R . . . .
C1 C 0.2646(3) 0.3354(2) 0.5515(2) 0.0286(8) Uani 1 1 d . . . . .
C2 C 0.2437(3) 0.3670(2) 0.4769(2) 0.0292(8) Uani 1 1 d . . . . .
C3 C 0.1544(3) 0.4444(2) 0.4618(2) 0.0321(8) Uani 1 1 d . . . . .
H3 H 0.110611 0.483713 0.498493 0.039 Uiso 1 1 calc R . . . .
C4 C 0.1277(3) 0.4656(3) 0.3935(2) 0.0319(8) Uani 1 1 d . . . . .
H4 H 0.065730 0.518266 0.383771 0.038 Uiso 1 1 calc R . . . .
C5 C 0.1936(3) 0.4081(2) 0.34050(19) 0.0286(8) Uani 1 1 d . . . . .
C6 C 0.2900(3) 0.3356(3) 0.3518(2) 0.0332(9) Uani 1 1 d . . . . .
H6 H 0.338261 0.299984 0.313486 0.040 Uiso 1 1 calc R . . . .
C7 C 0.3149(3) 0.3158(3) 0.4196(2) 0.0325(8) Uani 1 1 d . . . . .
H7 H 0.381628 0.266544 0.427596 0.039 Uiso 1 1 calc R . . . .
C8 C 0.1648(3) 0.3494(3) 0.2374(2) 0.0361(9) Uani 1 1 d . . . . .
H8 H 0.194821 0.284265 0.251996 0.043 Uiso 1 1 calc R . . . .
C9 C 0.1110(3) 0.5052(3) 0.2337(2) 0.0365(9) Uani 1 1 d . . . . .
H9 H 0.096756 0.567144 0.245841 0.044 Uiso 1 1 calc R . . . .
C10 C 0.0884(4) 0.4817(3) 0.1756(2) 0.0383(9) Uani 1 1 d . . . . .
H10 H 0.055476 0.524343 0.138957 0.046 Uiso 1 1 calc R . . . .
C11 C 0.1126(4) 0.3283(3) 0.1255(2) 0.0422(10) Uani 1 1 d . . . . .
H11A H 0.191636 0.313955 0.089490 0.051 Uiso 1 1 calc R . . . .
H11B H 0.051718 0.365499 0.098742 0.051 Uiso 1 1 calc R . . . .
C12 C 0.0758(4) 0.2369(3) 0.1654(2) 0.0380(9) Uani 1 1 d . . . . .
C13 C -0.0405(4) 0.2376(3) 0.2087(3) 0.0475(11) Uani 1 1 d . . . . .
H13 H -0.100295 0.294810 0.209401 0.057 Uiso 1 1 calc R . . . .
C14 C -0.0706(4) 0.1556(3) 0.2512(2) 0.0428(10) Uani 1 1 d . . . . .
H14 H -0.150849 0.156920 0.280386 0.051 Uiso 1 1 calc R . . . .
C15 C 0.0155(3) 0.0720(3) 0.2514(2) 0.0342(9) Uani 1 1 d . . . . .
C16 C 0.1308(4) 0.0705(3) 0.2047(2) 0.0412(10) Uani 1 1 d . . . . .
H16 H 0.189153 0.012481 0.201819 0.049 Uiso 1 1 calc R . . . .
C17 C 0.1613(4) 0.1521(3) 0.1628(2) 0.0414(10) Uani 1 1 d . . . . .
H17 H 0.240733 0.150249 0.132159 0.050 Uiso 1 1 calc R . . . .
C18 C -0.0073(3) -0.0143(3) 0.3043(2) 0.0326(9) Uani 1 1 d . . . . .
H18A H -0.093766 -0.004762 0.331123 0.039 Uiso 1 1 calc R . . . .
H18B H 0.012729 -0.069580 0.277745 0.039 Uiso 1 1 calc R . . . .
C19 C 0.0699(3) 0.0344(2) 0.3942(2) 0.0287(8) Uani 1 1 d . . . . .
H19 H 0.019370 0.096053 0.394116 0.034 Uiso 1 1 calc R . . . .
C20 C 0.1563(3) -0.1109(3) 0.3694(2) 0.0334(9) Uani 1 1 d . . . . .
H20 H 0.175039 -0.168114 0.349027 0.040 Uiso 1 1 calc R . . . .
C21 C 0.2098(3) -0.0922(2) 0.4167(2) 0.0307(8) Uani 1 1 d . . . . .
H21 H 0.273588 -0.133536 0.435559 0.037 Uiso 1 1 calc R . . . .
C22 C 0.1845(3) 0.0533(2) 0.4765(2) 0.0283(8) Uani 1 1 d . . . . .
C23 C 0.0988(3) 0.1308(2) 0.50229(19) 0.0294(8) Uani 1 1 d . . . . .
H23 H 0.019273 0.143279 0.495655 0.035 Uiso 1 1 calc R . . . .
C24 C 0.1301(3) 0.1897(3) 0.5378(2) 0.0304(8) Uani 1 1 d . . . . .
H24 H 0.071133 0.242585 0.555985 0.037 Uiso 1 1 calc R . . . .
C25 C 0.2472(3) 0.1727(2) 0.5475(2) 0.0309(8) Uani 1 1 d . . . . .
C26 C 0.3284(3) 0.0908(3) 0.5251(2) 0.0404(10) Uani 1 1 d . . . . .
H26 H 0.406009 0.075083 0.535017 0.048 Uiso 1 1 calc R . . . .
C27 C 0.2986(3) 0.0313(3) 0.4886(2) 0.0378(10) Uani 1 1 d . . . . .
H27 H 0.355844 -0.023358 0.472416 0.045 Uiso 1 1 calc R . . . .
C28 C 0.2803(3) 0.2422(2) 0.5803(2) 0.0295(8) Uani 1 1 d . . . . .
C29 C 0.3336(3) 0.2047(2) 0.6441(2) 0.0301(8) Uani 1 1 d . . . . .
C30 C 0.4436(3) 0.2266(2) 0.6424(2) 0.0308(8) Uani 1 1 d . . . . .
H30 H 0.482785 0.263181 0.600308 0.037 Uiso 1 1 calc R . . . .
C31 C 0.4953(3) 0.1956(2) 0.7010(2) 0.0305(8) Uani 1 1 d . . . . .
H31 H 0.569381 0.210760 0.699659 0.037 Uiso 1 1 calc R . . . .
C32 C 0.4375(3) 0.1420(2) 0.7617(2) 0.0297(8) Uani 1 1 d . . . . .
C33 C 0.3310(4) 0.1169(3) 0.7644(2) 0.0378(9) Uani 1 1 d . . . . .
H33 H 0.293247 0.079087 0.806140 0.045 Uiso 1 1 calc R . . . .
C34 C 0.2805(4) 0.1479(3) 0.7052(2) 0.0386(9) Uani 1 1 d . . . . .
H34 H 0.208254 0.130078 0.706184 0.046 Uiso 1 1 calc R . . . .
C35 C 0.5187(3) 0.1775(3) 0.8541(2) 0.0326(9) Uani 1 1 d . . . . .
H35 H 0.504093 0.244119 0.840147 0.039 Uiso 1 1 calc R . . . .
C36 C 0.5256(3) 0.0255(3) 0.8591(2) 0.0356(9) Uani 1 1 d . . . . .
H36 H 0.516307 -0.032051 0.848740 0.043 Uiso 1 1 calc R . . . .
C37 C 0.5753(3) 0.0353(3) 0.9112(2) 0.0343(9) Uani 1 1 d . . . . .
H37 H 0.607763 -0.014203 0.944492 0.041 Uiso 1 1 calc R . . . .
C38 C 0.6131(4) 0.1744(3) 0.9560(2) 0.0403(10) Uani 1 1 d . . . . .
H38A H 0.702694 0.157573 0.944796 0.048 Uiso 1 1 calc R . . . .
H38B H 0.581226 0.149486 1.007647 0.048 Uiso 1 1 calc R . . . .
C39 C 0.5713(3) 0.2799(3) 0.9451(2) 0.0348(9) Uani 1 1 d . . . . .
C40 C 0.4584(4) 0.3226(3) 0.9845(2) 0.0386(9) Uani 1 1 d . . . . .
H40 H 0.411915 0.285495 1.022514 0.046 Uiso 1 1 calc R . . . .
C41 C 0.4129(4) 0.4181(3) 0.9693(2) 0.0406(10) Uani 1 1 d . . . . .
H41 H 0.334957 0.445768 0.996665 0.049 Uiso 1 1 calc R . . . .
C42 C 0.4789(4) 0.4742(3) 0.9148(2) 0.0377(9) Uani 1 1 d . . . . .
C43 C 0.5935(4) 0.4321(3) 0.8774(3) 0.0513(11) Uani 1 1 d . . . . .
H43 H 0.641390 0.469619 0.840701 0.062 Uiso 1 1 calc R . . . .
C44 C 0.6393(4) 0.3361(3) 0.8928(3) 0.0497(11) Uani 1 1 d . . . . .
H44 H 0.718484 0.308716 0.866866 0.060 Uiso 1 1 calc R . . . .
C45 C 0.4242(4) 0.5763(3) 0.8939(2) 0.0452(11) Uani 1 1 d . . . . .
H45A H 0.348460 0.596385 0.931146 0.054 Uiso 1 1 calc R . . . .
H45B H 0.481055 0.616008 0.892189 0.054 Uiso 1 1 calc R . . . .
C46 C 0.3614(4) 0.5282(3) 0.7951(2) 0.0376(9) Uani 1 1 d . . . . .
H46 H 0.348819 0.467720 0.819538 0.045 Uiso 1 1 calc R . . . .
C47 C 0.4048(3) 0.6691(3) 0.7704(2) 0.0357(9) Uani 1 1 d . . . . .
H47 H 0.427691 0.724199 0.775366 0.043 Uiso 1 1 calc R . . . .
C48 C 0.3735(3) 0.6545(3) 0.7119(2) 0.0360(9) Uani 1 1 d . . . . .
H48 H 0.371042 0.696826 0.667986 0.043 Uiso 1 1 calc R . . . .
C49 C 0.3139(3) 0.5169(2) 0.6818(2) 0.0292(8) Uani 1 1 d . . . . .
C50 C 0.3670(3) 0.5276(2) 0.6068(2) 0.0315(8) Uani 1 1 d . . . . .
H50 H 0.417651 0.571595 0.585677 0.038 Uiso 1 1 calc R . . . .
C51 C 0.3446(3) 0.4733(2) 0.5639(2) 0.0304(8) Uani 1 1 d . . . . .
H51 H 0.379133 0.481288 0.512642 0.036 Uiso 1 1 calc R . . . .
C52 C 0.2722(3) 0.4064(2) 0.5940(2) 0.0281(8) Uani 1 1 d . . . . .
C53 C 0.2132(3) 0.4032(2) 0.6685(2) 0.0313(8) Uani 1 1 d . . . . .
H53 H 0.158175 0.362321 0.689278 0.038 Uiso 1 1 calc R . . . .
O3X O 0.6822(8) 0.0935(6) 0.3416(6) 0.064(3) Uani 0.367(7) 1 d D U P A 2
H3X H 0.712521 0.042529 0.364264 0.096 Uiso 0.367(7) 1 calc GR . P A 2
C56X C 0.5718(12) 0.0862(16) 0.3310(16) 0.058(4) Uani 0.367(7) 1 d D U P A 2
H56D H 0.574391 0.100435 0.278735 0.087 Uiso 0.367(7) 1 calc GR . P A 2
H56E H 0.505129 0.131256 0.357783 0.087 Uiso 0.367(7) 1 calc GR . P A 2
H56F H 0.559166 0.021757 0.349066 0.087 Uiso 0.367(7) 1 calc GR . P A 2
O1X O 0.7209(18) 0.1927(12) 0.0855(9) 0.139(5) Uani 0.367(7) 1 d D U P A 2
H1X H 0.783467 0.197586 0.051850 0.209 Uiso 0.367(7) 1 calc GR . P A 2
C54X C 0.746(3) 0.1110(15) 0.1349(12) 0.113(7) Uani 0.367(7) 1 d D U P A 2
H54D H 0.780161 0.056035 0.108352 0.170 Uiso 0.367(7) 1 calc GR . P A 2
H54E H 0.671363 0.101810 0.171410 0.170 Uiso 0.367(7) 1 calc GR . P A 2
H54F H 0.804811 0.118244 0.159476 0.170 Uiso 0.367(7) 1 calc GR . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 H1 0.8400 . ?
O1 C54 1.403(5) . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
O2 H2 0.8400 . ?
O2 C55 1.404(5) . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
O3 H3A 0.8400 . ?
O3 C56 1.405(5) . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
O6 H6A 0.8400 . ?
O6 C57 1.371(6) . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
O5 H5 0.8400 . ?
O5 C59 1.422(7) . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
O4 H4A 0.8400 . ?
O4 C021 1.411(6) . ?
C021 H02A 0.9800 . ?
C021 H02B 0.9800 . ?
C021 H02C 0.9800 . ?
N1 C5 1.445(4) . ?
N1 C8 1.343(5) . ?
N1 C9 1.391(5) . ?
N2 C8 1.321(5) . ?
N2 C10 1.383(5) . ?
N2 C11 1.488(4) . ?
N3 C18 1.482(4) . ?
N3 C19 1.327(4) . ?
N3 C20 1.378(4) . ?
N4 C19 1.344(4) . ?
N4 C21 1.388(4) . ?
N4 C22 1.443(4) . ?
N5 C32 1.441(4) . ?
N5 C35 1.338(4) . ?
N5 C36 1.383(4) . ?
N6 C35 1.329(4) . ?
N6 C37 1.378(5) . ?
N6 C38 1.497(4) . ?
N7 C45 1.482(5) . ?
N7 C46 1.333(4) . ?
N7 C47 1.375(5) . ?
N8 C46 1.331(5) . ?
N8 C48 1.393(4) . ?
N8 C49 1.437(4) . ?
C0AA H0AA 0.9500 . ?
C0AA C49 1.387(5) . ?
C0AA C53 1.381(5) . ?
C1 C2 1.490(5) . ?
C1 C28 1.364(5) . ?
C1 C52 1.487(5) . ?
C2 C3 1.387(5) . ?
C2 C7 1.402(5) . ?
C3 H3 0.9500 . ?
C3 C4 1.396(5) . ?
C4 H4 0.9500 . ?
C4 C5 1.384(5) . ?
C5 C6 1.381(5) . ?
C6 H6 0.9500 . ?
C6 C7 1.381(5) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C9 C10 1.348(5) . ?
C10 H10 0.9500 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.518(6) . ?
C12 C13 1.385(6) . ?
C12 C17 1.390(5) . ?
C13 H13 0.9500 . ?
C13 C14 1.387(6) . ?
C14 H14 0.9500 . ?
C14 C15 1.380(5) . ?
C15 C16 1.397(6) . ?
C15 C18 1.496(5) . ?
C16 H16 0.9500 . ?
C16 C17 1.379(6) . ?
C17 H17 0.9500 . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C20 C21 1.352(5) . ?
C21 H21 0.9500 . ?
C22 C23 1.384(5) . ?
C22 C27 1.379(5) . ?
C23 H23 0.9500 . ?
C23 C24 1.382(5) . ?
C24 H24 0.9500 . ?
C24 C25 1.400(5) . ?
C25 C26 1.392(5) . ?
C25 C28 1.487(5) . ?
C26 H26 0.9500 . ?
C26 C27 1.391(5) . ?
C27 H27 0.9500 . ?
C28 C29 1.487(5) . ?
C29 C30 1.407(5) . ?
C29 C34 1.392(5) . ?
C30 H30 0.9500 . ?
C30 C31 1.380(5) . ?
C31 H31 0.9500 . ?
C31 C32 1.383(5) . ?
C32 C33 1.385(5) . ?
C33 H33 0.9500 . ?
C33 C34 1.380(5) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C36 C37 1.347(5) . ?
C37 H37 0.9500 . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C38 C39 1.499(5) . ?
C39 C40 1.386(5) . ?
C39 C44 1.377(6) . ?
C40 H40 0.9500 . ?
C40 C41 1.377(5) . ?
C41 H41 0.9500 . ?
C41 C42 1.385(6) . ?
C42 C43 1.385(6) . ?
C42 C45 1.501(5) . ?
C43 H43 0.9500 . ?
C43 C44 1.385(6) . ?
C44 H44 0.9500 . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 H46 0.9500 . ?
C47 H47 0.9500 . ?
C47 C48 1.353(5) . ?
C48 H48 0.9500 . ?
C49 C50 1.394(5) . ?
C50 H50 0.9500 . ?
C50 C51 1.376(5) . ?
C51 H51 0.9500 . ?
C51 C52 1.402(5) . ?
C52 C53 1.401(5) . ?
C53 H53 0.9500 . ?
O3X H3X 0.8400 . ?
O3X C56X 1.409(5) . ?
C56X H56D 0.9800 . ?
C56X H56E 0.9800 . ?
C56X H56F 0.9800 . ?
O1X H1X 0.8400 . ?
O1X C54X 1.404(5) . ?
C54X H54D 0.9800 . ?
C54X H54E 0.9800 . ?
C54X H54F 0.9800 . ?

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
C54 O1 H1 109.5 . . ?
O1 C54 H54A 109.5 . . ?
O1 C54 H54B 109.5 . . ?
O1 C54 H54C 109.5 . . ?
H54A C54 H54B 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C55 O2 H2 109.5 . . ?
O2 C55 H55A 109.5 . . ?
O2 C55 H55B 109.5 . . ?
O2 C55 H55C 109.5 . . ?
H55A C55 H55B 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C56 O3 H3A 109.5 . . ?
O3 C56 H56A 109.5 . . ?
O3 C56 H56B 109.5 . . ?
O3 C56 H56C 109.5 . . ?
H56A C56 H56B 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C57 O6 H6A 109.5 . . ?
O6 C57 H57A 109.5 . . ?
O6 C57 H57B 109.5 . . ?
O6 C57 H57C 109.5 . . ?
H57A C57 H57B 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C59 O5 H5 109.5 . . ?
O5 C59 H59A 109.5 . . ?
O5 C59 H59B 109.5 . . ?
O5 C59 H59C 109.5 . . ?
H59A C59 H59B 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C021 O4 H4A 109.5 . . ?
O4 C021 H02A 109.5 . . ?
O4 C021 H02B 109.5 . . ?
O4 C021 H02C 109.5 . . ?
H02A C021 H02B 109.5 . . ?
H02A C021 H02C 109.5 . . ?
H02B C021 H02C 109.5 . . ?
C8 N1 C5 123.7(3) . . ?
C8 N1 C9 108.2(3) . . ?
C9 N1 C5 128.1(3) . . ?
C8 N2 C10 108.7(3) . . ?
C8 N2 C11 125.7(3) . . ?
C10 N2 C11 125.6(3) . . ?
C19 N3 C18 122.8(3) . . ?
C19 N3 C20 109.2(3) . . ?
C20 N3 C18 127.8(3) . . ?
C19 N4 C21 108.3(3) . . ?
C19 N4 C22 123.5(3) . . ?
C21 N4 C22 128.0(3) . . ?
C35 N5 C32 123.0(3) . . ?
C35 N5 C36 108.4(3) . . ?
C36 N5 C32 128.5(3) . . ?
C35 N6 C37 108.8(3) . . ?
C35 N6 C38 125.2(3) . . ?
C37 N6 C38 126.0(3) . . ?
C46 N7 C45 126.1(3) . . ?
C46 N7 C47 108.6(3) . . ?
C47 N7 C45 125.3(3) . . ?
C46 N8 C48 108.5(3) . . ?
C46 N8 C49 124.5(3) . . ?
C48 N8 C49 126.9(3) . . ?
C49 C0AA H0AA 120.5 . . ?
C53 C0AA H0AA 120.5 . . ?
C53 C0AA C49 118.9(3) . . ?
C28 C1 C2 121.0(3) . . ?
C28 C1 C52 119.7(3) . . ?
C52 C1 C2 119.3(3) . . ?
C3 C2 C1 122.7(3) . . ?
C3 C2 C7 118.1(3) . . ?
C7 C2 C1 119.2(3) . . ?
C2 C3 H3 119.4 . . ?
C2 C3 C4 121.2(3) . . ?
C4 C3 H3 119.4 . . ?
C3 C4 H4 120.8 . . ?
C5 C4 C3 118.5(3) . . ?
C5 C4 H4 120.8 . . ?
C4 C5 N1 119.9(3) . . ?
C6 C5 N1 118.4(3) . . ?
C6 C5 C4 121.6(3) . . ?
C5 C6 H6 120.6 . . ?
C7 C6 C5 118.8(3) . . ?
C7 C6 H6 120.6 . . ?
C2 C7 H7 119.3 . . ?
C6 C7 C2 121.3(3) . . ?
C6 C7 H7 119.3 . . ?
N1 C8 H8 125.6 . . ?
N2 C8 N1 108.8(3) . . ?
N2 C8 H8 125.6 . . ?
N1 C9 H9 126.7 . . ?
C10 C9 N1 106.7(3) . . ?
C10 C9 H9 126.7 . . ?
N2 C10 H10 126.2 . . ?
C9 C10 N2 107.6(3) . . ?
C9 C10 H10 126.2 . . ?
N2 C11 H11A 109.8 . . ?
N2 C11 H11B 109.8 . . ?
N2 C11 C12 109.6(3) . . ?
H11A C11 H11B 108.2 . . ?
C12 C11 H11A 109.8 . . ?
C12 C11 H11B 109.8 . . ?
C13 C12 C11 120.7(4) . . ?
C13 C12 C17 119.2(4) . . ?
C17 C12 C11 120.0(4) . . ?
C12 C13 H13 119.7 . . ?
C12 C13 C14 120.7(4) . . ?
C14 C13 H13 119.7 . . ?
C13 C14 H14 119.8 . . ?
C15 C14 C13 120.4(4) . . ?
C15 C14 H14 119.8 . . ?
C14 C15 C16 118.7(4) . . ?
C14 C15 C18 122.2(4) . . ?
C16 C15 C18 118.9(3) . . ?
C15 C16 H16 119.5 . . ?
C17 C16 C15 121.0(4) . . ?
C17 C16 H16 119.5 . . ?
C12 C17 H17 120.0 . . ?
C16 C17 C12 119.9(4) . . ?
C16 C17 H17 120.0 . . ?
N3 C18 C15 108.5(3) . . ?
N3 C18 H18A 110.0 . . ?
N3 C18 H18B 110.0 . . ?
C15 C18 H18A 110.0 . . ?
C15 C18 H18B 110.0 . . ?
H18A C18 H18B 108.4 . . ?
N3 C19 N4 108.3(3) . . ?
N3 C19 H19 125.9 . . ?
N4 C19 H19 125.9 . . ?
N3 C20 H20 126.4 . . ?
C21 C20 N3 107.2(3) . . ?
C21 C20 H20 126.4 . . ?
N4 C21 H21 126.5 . . ?
C20 C21 N4 107.0(3) . . ?
C20 C21 H21 126.5 . . ?
C23 C22 N4 118.3(3) . . ?
C27 C22 N4 120.5(3) . . ?
C27 C22 C23 121.1(3) . . ?
C22 C23 H23 120.3 . . ?
C24 C23 C22 119.4(3) . . ?
C24 C23 H23 120.3 . . ?
C23 C24 H24 119.5 . . ?
C23 C24 C25 121.0(3) . . ?
C25 C24 H24 119.5 . . ?
C24 C25 C28 119.4(3) . . ?
C26 C25 C24 117.9(3) . . ?
C26 C25 C28 122.7(3) . . ?
C25 C26 H26 119.2 . . ?
C27 C26 C25 121.6(3) . . ?
C27 C26 H26 119.2 . . ?
C22 C27 C26 118.8(3) . . ?
C22 C27 H27 120.6 . . ?
C26 C27 H27 120.6 . . ?
C1 C28 C25 120.9(3) . . ?
C1 C28 C29 122.1(3) . . ?
C25 C28 C29 116.9(3) . . ?
C30 C29 C28 118.6(3) . . ?
C34 C29 C28 123.0(3) . . ?
C34 C29 C30 118.4(3) . . ?
C29 C30 H30 119.6 . . ?
C31 C30 C29 120.8(4) . . ?
C31 C30 H30 119.6 . . ?
C30 C31 H31 120.5 . . ?
C30 C31 C32 119.0(3) . . ?
C32 C31 H31 120.5 . . ?
C31 C32 N5 117.4(3) . . ?
C31 C32 C33 121.6(3) . . ?
C33 C32 N5 120.9(3) . . ?
C32 C33 H33 120.6 . . ?
C34 C33 C32 118.8(4) . . ?
C34 C33 H33 120.6 . . ?
C29 C34 H34 119.4 . . ?
C33 C34 C29 121.2(4) . . ?
C33 C34 H34 119.4 . . ?
N5 C35 H35 125.8 . . ?
N6 C35 N5 108.4(3) . . ?
N6 C35 H35 125.8 . . ?
N5 C36 H36 126.5 . . ?
C37 C36 N5 107.0(3) . . ?
C37 C36 H36 126.5 . . ?
N6 C37 H37 126.3 . . ?
C36 C37 N6 107.3(3) . . ?
C36 C37 H37 126.3 . . ?
N6 C38 H38A 109.5 . . ?
N6 C38 H38B 109.5 . . ?
N6 C38 C39 110.6(3) . . ?
H38A C38 H38B 108.1 . . ?
C39 C38 H38A 109.5 . . ?
C39 C38 H38B 109.5 . . ?
C40 C39 C38 120.2(4) . . ?
C44 C39 C38 121.3(4) . . ?
C44 C39 C40 118.4(4) . . ?
C39 C40 H40 119.6 . . ?
C41 C40 C39 120.9(4) . . ?
C41 C40 H40 119.6 . . ?
C40 C41 H41 119.5 . . ?
C40 C41 C42 121.0(4) . . ?
C42 C41 H41 119.5 . . ?
C41 C42 C43 118.0(4) . . ?
C41 C42 C45 120.6(4) . . ?
C43 C42 C45 121.2(4) . . ?
C42 C43 H43 119.5 . . ?
C44 C43 C42 120.9(4) . . ?
C44 C43 H43 119.5 . . ?
C39 C44 C43 120.7(4) . . ?
C39 C44 H44 119.6 . . ?
C43 C44 H44 119.6 . . ?
N7 C45 C42 110.3(3) . . ?
N7 C45 H45A 109.6 . . ?
N7 C45 H45B 109.6 . . ?
C42 C45 H45A 109.6 . . ?
C42 C45 H45B 109.6 . . ?
H45A C45 H45B 108.1 . . ?
N7 C46 H46 125.6 . . ?
N8 C46 N7 108.8(3) . . ?
N8 C46 H46 125.6 . . ?
N7 C47 H47 126.2 . . ?
C48 C47 N7 107.6(3) . . ?
C48 C47 H47 126.2 . . ?
N8 C48 H48 126.7 . . ?
C47 C48 N8 106.5(3) . . ?
C47 C48 H48 126.7 . . ?
C0AA C49 N8 119.0(3) . . ?
C0AA C49 C50 121.0(3) . . ?
C50 C49 N8 119.9(3) . . ?
C49 C50 H50 120.6 . . ?
C51 C50 C49 118.9(3) . . ?
C51 C50 H50 120.6 . . ?
C50 C51 H51 119.2 . . ?
C50 C51 C52 121.6(3) . . ?
C52 C51 H51 119.2 . . ?
C51 C52 C1 122.5(3) . . ?
C53 C52 C1 119.8(3) . . ?
C53 C52 C51 117.5(3) . . ?
C0AA C53 C52 121.6(3) . . ?
C0AA C53 H53 119.2 . . ?
C52 C53 H53 119.2 . . ?
C56X O3X H3X 109.5 . . ?
O3X C56X H56D 109.5 . . ?
O3X C56X H56E 109.5 . . ?
O3X C56X H56F 109.5 . . ?
H56D C56X H56E 109.5 . . ?
H56D C56X H56F 109.5 . . ?
H56E C56X H56F 109.5 . . ?
C54X O1X H1X 109.5 . . ?
O1X C54X H54D 109.5 . . ?
O1X C54X H54E 109.5 . . ?
O1X C54X H54F 109.5 . . ?
H54D C54X H54E 109.5 . . ?
H54D C54X H54F 109.5 . . ?
H54E C54X H54F 109.5 . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.500 0.000 171.1 54.2 3(CH4O)
2 0.312 0.084 0.302 22.4 7.2 ?
3 0.688 -0.084 0.698 22.4 7.1 ?

_olex2_submission_special_instructions 'No special instructions were received'
