# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_Mg_dmpu5_I2
_database_code_depnum_ccdc_archive 'CCDC 2206123'
loop_
_audit_author_name
_audit_author_address
'Lars Eriksson'
;Stockholm University
Sweden
;
_audit_update_record             
;
2022-09-08 deposited with the CCDC.	2023-12-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H60 Mg N10 O5, 2(I)'
_chemical_formula_sum            'C30 H60 I2 Mg N10 O5'
_chemical_formula_weight         918.99

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'
I I -0.3257 6.8362 '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'
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'

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

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

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

_cell_length_a                   15.03480(19)
_cell_length_b                   20.2696(2)
_cell_length_c                   14.7659(2)
_cell_angle_alpha                90
_cell_angle_beta                 116.7976(17)
_cell_angle_gamma                90
_cell_volume                     4016.62(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    20462
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      69.3860
_cell_measurement_theta_min      3.9450

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_F_000             1872
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    12.846
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?

_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45329
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.0131
_diffrn_reflns_number            42715
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.293
_diffrn_reflns_theta_max         69.454
_diffrn_reflns_theta_full        67.684
_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 0.995
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             7489
_reflns_number_gt                7056
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _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_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_structure_solution    'SHELXS-97(Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0279P)²+3.4318P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7489
_refine_ls_number_parameters     443
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0244
_refine_ls_R_factor_gt           0.0224
_refine_ls_wR_factor_ref         0.0566
_refine_ls_wR_factor_gt          0.0556
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.80336(2) 0.63528(2) 0.79908(2) 0.01387(5) Uani 1 1 d . . . . .
Mg1 Mg 0.75026(5) 0.51485(3) 0.23785(5) 0.00753(13) Uani 1 1 d . . . . .
O2 O 0.83153(12) 0.52515(8) 0.38704(12) 0.0163(3) Uani 1 1 d . . . . .
O3 O 0.65981(11) 0.58523(7) 0.15150(11) 0.0112(3) Uani 1 1 d . . . . .
O1 O 0.63541(11) 0.47956(8) 0.25944(13) 0.0150(3) Uani 1 1 d . . . . .
O5 O 0.76561(10) 0.42848(7) 0.18518(12) 0.0120(3) Uani 1 1 d . . . . .
O4 O 0.86185(11) 0.55286(7) 0.21229(12) 0.0128(3) Uani 1 1 d . . . . .
N6 N 0.63357(13) 0.69441(9) 0.11929(14) 0.0099(4) Uani 1 1 d . . . . .
N1 N 0.50778(13) 0.50056(9) 0.29726(15) 0.0124(4) Uani 1 1 d . . . . .
N9 N 0.69140(13) 0.37319(9) 0.03615(15) 0.0124(4) Uani 1 1 d . . . . .
N10 N 0.86273(13) 0.36557(9) 0.13914(14) 0.0112(4) Uani 1 1 d . . . . .
N2 N 0.58847(13) 0.39891(9) 0.33550(14) 0.0128(4) Uani 1 1 d . . . . .
N4 N 0.86975(14) 0.44204(10) 0.50091(15) 0.0176(4) Uani 1 1 d . . . . .
N5 N 0.64928(13) 0.62388(9) 0.00253(14) 0.0109(4) Uani 1 1 d . . . . .
C4 C 0.51991(17) 0.37202(11) 0.37174(18) 0.0144(4) Uani 1 1 d . . . . .
H4A H 0.555693 0.339944 0.426883 0.017 Uiso 1 1 calc R U . . .
H4B H 0.464921 0.348452 0.315663 0.017 Uiso 1 1 calc R U . . .
C1 C 0.57901(15) 0.46001(10) 0.29571(16) 0.0101(4) Uani 1 1 d . . . . .
N8 N 0.90609(14) 0.66042(9) 0.21698(15) 0.0141(4) Uani 1 1 d . . . . .
N3 N 0.77937(14) 0.53187(10) 0.50922(15) 0.0158(4) Uani 1 1 d . . . . .
C19 C 0.89946(14) 0.59781(11) 0.18232(16) 0.0101(4) Uani 1 1 d . . . . .
C16 C 0.60942(16) 0.75168(10) 0.05124(17) 0.0126(4) Uani 1 1 d . . . . .
H16A H 0.638216 0.792053 0.091639 0.015 Uiso 1 1 calc R U . . .
H16B H 0.536214 0.757271 0.014643 0.015 Uiso 1 1 calc R U . . .
C13 C 0.64797(14) 0.63291(10) 0.09255(16) 0.0082(4) Uani 1 1 d . . . . .
N7 N 0.93472(13) 0.58477(9) 0.11444(14) 0.0129(4) Uani 1 1 d . . . . .
C25 C 0.77268(15) 0.38964(10) 0.12233(17) 0.0087(4) Uani 1 1 d . . . . .
C21 C 0.95108(19) 0.70115(12) 0.0864(2) 0.0225(5) Uani 1 1 d . . . . .
H21A H 0.882409 0.704266 0.030775 0.027 Uiso 1 1 calc R U . . .
H21B H 0.992780 0.734217 0.073961 0.027 Uiso 1 1 calc R U . . .
C18 C 0.61936(16) 0.70432(11) 0.20960(17) 0.0129(4) Uani 1 1 d . . . . .
H18A H 0.654775 0.744239 0.244992 0.019 Uiso 1 1 calc R U . . .
H18B H 0.645619 0.666177 0.254726 0.019 Uiso 1 1 calc R U . . .
H18C H 0.548121 0.709210 0.189855 0.019 Uiso 1 1 calc R U . . .
C29 C 0.59326(15) 0.38415(12) 0.03090(19) 0.0170(5) Uani 1 1 d . . . . .
H29A H 0.569987 0.343367 0.048905 0.025 Uiso 1 1 calc R U . . .
H29B H 0.546299 0.397261 -0.038189 0.025 Uiso 1 1 calc R U . . .
H29C H 0.597589 0.419185 0.078456 0.025 Uiso 1 1 calc R U . . .
C5 C 0.48377(17) 0.56202(11) 0.24056(19) 0.0170(5) Uani 1 1 d . . . . .
H5A H 0.534761 0.571541 0.218296 0.026 Uiso 1 1 calc R U . . .
H5B H 0.481716 0.597959 0.283984 0.026 Uiso 1 1 calc R U . . .
H5C H 0.418628 0.558032 0.181169 0.026 Uiso 1 1 calc R U . . .
C30 C 0.94919(16) 0.38107(12) 0.23447(18) 0.0163(5) Uani 1 1 d . . . . .
H30A H 0.943562 0.426357 0.254539 0.024 Uiso 1 1 calc R U . . .
H30B H 1.009868 0.376848 0.225852 0.024 Uiso 1 1 calc R U . . .
H30C H 0.952331 0.350426 0.287168 0.024 Uiso 1 1 calc R U . . .
C7 C 0.82640(15) 0.50006(11) 0.46325(16) 0.0120(4) Uani 1 1 d . . . . .
C28 C 0.87294(17) 0.31311(12) 0.07650(18) 0.0175(5) Uani 1 1 d . . . . .
H28A H 0.863772 0.269624 0.101649 0.021 Uiso 1 1 calc R U . . .
H28B H 0.940538 0.314422 0.080742 0.021 Uiso 1 1 calc R U . . .
C15 C 0.65047(17) 0.74239(11) -0.02437(18) 0.0161(5) Uani 1 1 d . . . . .
H15A H 0.624650 0.777544 -0.076426 0.019 Uiso 1 1 calc R U . . .
H15B H 0.724048 0.745764 0.010769 0.019 Uiso 1 1 calc R U . . .
C8 C 0.76263(17) 0.50080(12) 0.58981(17) 0.0172(5) Uani 1 1 d . . . . .
H8A H 0.702728 0.472365 0.559517 0.021 Uiso 1 1 calc R U . . .
H8B H 0.751154 0.535188 0.630998 0.021 Uiso 1 1 calc R U . . .
C20 C 0.99194(17) 0.63296(12) 0.08872(19) 0.0189(5) Uani 1 1 d . . . . .
H20A H 0.987923 0.622298 0.021550 0.023 Uiso 1 1 calc R U . . .
H20B H 1.062829 0.631252 0.139679 0.023 Uiso 1 1 calc R U . . .
C2 C 0.43403(16) 0.47933(11) 0.33034(18) 0.0145(4) Uani 1 1 d . . . . .
H2A H 0.374344 0.461957 0.271576 0.017 Uiso 1 1 calc R U . . .
H2B H 0.413317 0.517525 0.358145 0.017 Uiso 1 1 calc R U . . .
C14 C 0.62032(16) 0.67572(11) -0.07472(17) 0.0138(4) Uani 1 1 d . . . . .
H14A H 0.547312 0.674564 -0.117723 0.017 Uiso 1 1 calc R U . . .
H14B H 0.653152 0.667999 -0.118744 0.017 Uiso 1 1 calc R U . . .
C17 C 0.65192(18) 0.55734(11) -0.03365(18) 0.0175(5) Uani 1 1 d . . . . .
H17A H 0.689937 0.528495 0.024333 0.026 Uiso 1 1 calc R U . . .
H17B H 0.683823 0.558281 -0.078692 0.026 Uiso 1 1 calc R U . . .
H17C H 0.583774 0.540522 -0.070920 0.026 Uiso 1 1 calc R U . . .
C10 C 0.87091(19) 0.41062(13) 0.59111(19) 0.0223(5) Uani 1 1 d . . . . .
H10A H 0.936485 0.389461 0.631219 0.027 Uiso 1 1 calc R U . . .
H10B H 0.819231 0.375806 0.569627 0.027 Uiso 1 1 calc R U . . .
C3 C 0.47754(17) 0.42647(12) 0.41052(18) 0.0160(5) Uani 1 1 d . . . . .
H3A H 0.425105 0.408470 0.426611 0.019 Uiso 1 1 calc R U . . .
H3B H 0.530754 0.445513 0.473325 0.019 Uiso 1 1 calc R U . . .
C22 C 0.9508(2) 0.71497(12) 0.18699(19) 0.0234(5) Uani 1 1 d . . . . .
H22A H 1.020056 0.721863 0.239816 0.028 Uiso 1 1 calc R U . . .
H22B H 0.912810 0.755926 0.181519 0.028 Uiso 1 1 calc R U . . .
C26 C 0.69415(17) 0.32366(11) -0.03506(17) 0.0156(5) Uani 1 1 d . . . . .
H26A H 0.642926 0.334239 -0.104588 0.019 Uiso 1 1 calc R U . . .
H26B H 0.678756 0.279633 -0.016695 0.019 Uiso 1 1 calc R U . . .
C9 C 0.85186(17) 0.46006(12) 0.65622(17) 0.0183(5) Uani 1 1 d . . . . .
H9A H 0.839370 0.436976 0.708473 0.022 Uiso 1 1 calc R U . . .
H9B H 0.910795 0.488891 0.690999 0.022 Uiso 1 1 calc R U . . .
C24 C 0.88271(16) 0.67558(12) 0.30046(18) 0.0162(5) Uani 1 1 d . . . . .
H24A H 0.864635 0.634877 0.324001 0.024 Uiso 1 1 calc R U . . .
H24B H 0.826738 0.706583 0.277094 0.024 Uiso 1 1 calc R U . . .
H24C H 0.941053 0.695455 0.356375 0.024 Uiso 1 1 calc R U . . .
C12 C 0.9204(2) 0.40633(15) 0.4518(2) 0.0295(6) Uani 1 1 d . . . . .
H12A H 0.896206 0.422040 0.381943 0.044 Uiso 1 1 calc R U . . .
H12B H 0.906605 0.359042 0.451357 0.044 Uiso 1 1 calc R U . . .
H12C H 0.992337 0.413909 0.489225 0.044 Uiso 1 1 calc R U . . .
C27 C 0.79564(17) 0.32224(12) -0.03256(18) 0.0188(5) Uani 1 1 d . . . . .
H27A H 0.807786 0.364068 -0.059799 0.023 Uiso 1 1 calc R U . . .
H27B H 0.799428 0.285445 -0.074771 0.023 Uiso 1 1 calc R U . . .
C11 C 0.7322(2) 0.59534(13) 0.4718(2) 0.0255(6) Uani 1 1 d . . . . .
H11A H 0.759859 0.615314 0.429552 0.038 Uiso 1 1 calc R U . . .
H11B H 0.744661 0.624420 0.529343 0.038 Uiso 1 1 calc R U . . .
H11C H 0.660246 0.589118 0.431331 0.038 Uiso 1 1 calc R U . . .
C23 C 0.92896(18) 0.51854(12) 0.07467(19) 0.0181(5) Uani 1 1 d . . . . .
H23A H 0.994905 0.497857 0.107403 0.027 Uiso 1 1 calc R U . . .
H23B H 0.906418 0.520728 0.001263 0.027 Uiso 1 1 calc R U . . .
H23C H 0.881651 0.492341 0.088489 0.027 Uiso 1 1 calc R U . . .
C6 C 0.65751(17) 0.35157(11) 0.32736(19) 0.0172(5) Uani 1 1 d . . . . .
H6A H 0.702720 0.335041 0.395035 0.026 Uiso 1 1 calc R U . . .
H6B H 0.696261 0.373203 0.297374 0.026 Uiso 1 1 calc R U . . .
H6C H 0.619961 0.314654 0.284205 0.026 Uiso 1 1 calc R U . . .
I2 I 0.68077(2) 0.30734(2) 0.66541(2) 0.02447(5) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mg1 O5 1.9711(16) . ?
Mg1 O3 1.9865(16) . ?
Mg1 O2 1.9907(17) . ?
Mg1 O1 2.0227(16) . ?
Mg1 O4 2.0302(15) . ?
O2 C7 1.269(3) . ?
O3 C13 1.258(3) . ?
O1 C1 1.254(3) . ?
O5 C25 1.257(3) . ?
O4 C19 1.254(3) . ?
N6 C13 1.354(3) . ?
N6 C18 1.456(3) . ?
N6 C16 1.470(3) . ?
N1 C1 1.358(3) . ?
N1 C5 1.453(3) . ?
N1 C2 1.463(3) . ?
N9 C25 1.350(3) . ?
N9 C29 1.459(3) . ?
N9 C26 1.468(3) . ?
N10 C25 1.353(3) . ?
N10 C30 1.456(3) . ?
N10 C28 1.462(3) . ?
N2 C1 1.351(3) . ?
N2 C6 1.458(3) . ?
N2 C4 1.464(3) . ?
N4 C7 1.338(3) . ?
N4 C12 1.458(3) . ?
N4 C10 1.469(3) . ?
N5 C13 1.351(3) . ?
N5 C17 1.458(3) . ?
N5 C14 1.465(3) . ?
C4 C3 1.510(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
N8 C19 1.355(3) . ?
N8 C24 1.459(3) . ?
N8 C22 1.462(3) . ?
N3 C7 1.345(3) . ?
N3 C11 1.453(3) . ?
N3 C8 1.465(3) . ?
C19 N7 1.354(3) . ?
C16 C15 1.511(3) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
N7 C23 1.452(3) . ?
N7 C20 1.460(3) . ?
C21 C20 1.507(4) . ?
C21 C22 1.513(4) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C28 C27 1.513(3) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C15 C14 1.510(3) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C8 C9 1.502(3) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C2 C3 1.510(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C10 C9 1.503(3) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C26 C27 1.510(3) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 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
O5 Mg1 O3 123.55(7) . . ?
O5 Mg1 O2 114.02(7) . . ?
O3 Mg1 O2 122.41(7) . . ?
O5 Mg1 O1 90.47(7) . . ?
O3 Mg1 O1 88.23(7) . . ?
O2 Mg1 O1 90.25(7) . . ?
O5 Mg1 O4 90.58(6) . . ?
O3 Mg1 O4 89.55(7) . . ?
O2 Mg1 O4 91.12(7) . . ?
O1 Mg1 O4 177.77(7) . . ?
C7 O2 Mg1 133.41(14) . . ?
C13 O3 Mg1 146.91(13) . . ?
C1 O1 Mg1 165.65(16) . . ?
C25 O5 Mg1 155.66(15) . . ?
C19 O4 Mg1 152.08(14) . . ?
C13 N6 C18 120.17(18) . . ?
C13 N6 C16 123.39(18) . . ?
C18 N6 C16 115.10(17) . . ?
C1 N1 C5 120.15(18) . . ?
C1 N1 C2 123.33(18) . . ?
C5 N1 C2 114.56(17) . . ?
C25 N9 C29 118.46(18) . . ?
C25 N9 C26 122.57(18) . . ?
C29 N9 C26 114.86(18) . . ?
C25 N10 C30 118.88(18) . . ?
C25 N10 C28 121.88(18) . . ?
C30 N10 C28 117.77(17) . . ?
C1 N2 C6 120.46(18) . . ?
C1 N2 C4 123.16(18) . . ?
C6 N2 C4 115.47(18) . . ?
C7 N4 C12 119.7(2) . . ?
C7 N4 C10 124.21(19) . . ?
C12 N4 C10 116.1(2) . . ?
C13 N5 C17 120.06(18) . . ?
C13 N5 C14 122.54(18) . . ?
C17 N5 C14 115.20(18) . . ?
N2 C4 C3 110.69(18) . . ?
N2 C4 H4A 109.5 . . ?
C3 C4 H4A 109.5 . . ?
N2 C4 H4B 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 108.1 . . ?
O1 C1 N2 121.11(19) . . ?
O1 C1 N1 120.40(19) . . ?
N2 C1 N1 118.48(18) . . ?
C19 N8 C24 120.77(19) . . ?
C19 N8 C22 124.01(19) . . ?
C24 N8 C22 114.53(19) . . ?
C7 N3 C11 120.7(2) . . ?
C7 N3 C8 121.73(19) . . ?
C11 N3 C8 117.15(19) . . ?
O4 C19 N7 120.6(2) . . ?
O4 C19 N8 121.02(19) . . ?
N7 C19 N8 118.39(19) . . ?
N6 C16 C15 110.46(17) . . ?
N6 C16 H16A 109.6 . . ?
C15 C16 H16A 109.6 . . ?
N6 C16 H16B 109.6 . . ?
C15 C16 H16B 109.6 . . ?
H16A C16 H16B 108.1 . . ?
O3 C13 N5 121.09(19) . . ?
O3 C13 N6 119.78(19) . . ?
N5 C13 N6 119.13(18) . . ?
C19 N7 C23 120.51(18) . . ?
C19 N7 C20 122.34(19) . . ?
C23 N7 C20 116.61(18) . . ?
O5 C25 N9 120.57(18) . . ?
O5 C25 N10 120.07(19) . . ?
N9 C25 N10 119.32(19) . . ?
C20 C21 C22 109.2(2) . . ?
C20 C21 H21A 109.8 . . ?
C22 C21 H21A 109.8 . . ?
C20 C21 H21B 109.8 . . ?
C22 C21 H21B 109.8 . . ?
H21A C21 H21B 108.3 . . ?
N6 C18 H18A 109.5 . . ?
N6 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N6 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N9 C29 H29A 109.5 . . ?
N9 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
N9 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N1 C5 H5A 109.5 . . ?
N1 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N1 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N10 C30 H30A 109.5 . . ?
N10 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
N10 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
O2 C7 N4 120.5(2) . . ?
O2 C7 N3 120.8(2) . . ?
N4 C7 N3 118.7(2) . . ?
N10 C28 C27 109.57(18) . . ?
N10 C28 H28A 109.8 . . ?
C27 C28 H28A 109.8 . . ?
N10 C28 H28B 109.8 . . ?
C27 C28 H28B 109.8 . . ?
H28A C28 H28B 108.2 . . ?
C14 C15 C16 110.07(18) . . ?
C14 C15 H15A 109.6 . . ?
C16 C15 H15A 109.6 . . ?
C14 C15 H15B 109.6 . . ?
C16 C15 H15B 109.6 . . ?
H15A C15 H15B 108.2 . . ?
N3 C8 C9 109.67(18) . . ?
N3 C8 H8A 109.7 . . ?
C9 C8 H8A 109.7 . . ?
N3 C8 H8B 109.7 . . ?
C9 C8 H8B 109.7 . . ?
H8A C8 H8B 108.2 . . ?
N7 C20 C21 109.72(19) . . ?
N7 C20 H20A 109.7 . . ?
C21 C20 H20A 109.7 . . ?
N7 C20 H20B 109.7 . . ?
C21 C20 H20B 109.7 . . ?
H20A C20 H20B 108.2 . . ?
N1 C2 C3 110.17(18) . . ?
N1 C2 H2A 109.6 . . ?
C3 C2 H2A 109.6 . . ?
N1 C2 H2B 109.6 . . ?
C3 C2 H2B 109.6 . . ?
H2A C2 H2B 108.1 . . ?
N5 C14 C15 109.91(18) . . ?
N5 C14 H14A 109.7 . . ?
C15 C14 H14A 109.7 . . ?
N5 C14 H14B 109.7 . . ?
C15 C14 H14B 109.7 . . ?
H14A C14 H14B 108.2 . . ?
N5 C17 H17A 109.5 . . ?
N5 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
N5 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N4 C10 C9 111.3(2) . . ?
N4 C10 H10A 109.4 . . ?
C9 C10 H10A 109.4 . . ?
N4 C10 H10B 109.4 . . ?
C9 C10 H10B 109.4 . . ?
H10A C10 H10B 108.0 . . ?
C2 C3 C4 109.22(18) . . ?
C2 C3 H3A 109.8 . . ?
C4 C3 H3A 109.8 . . ?
C2 C3 H3B 109.8 . . ?
C4 C3 H3B 109.8 . . ?
H3A C3 H3B 108.3 . . ?
N8 C22 C21 111.2(2) . . ?
N8 C22 H22A 109.4 . . ?
C21 C22 H22A 109.4 . . ?
N8 C22 H22B 109.4 . . ?
C21 C22 H22B 109.4 . . ?
H22A C22 H22B 108.0 . . ?
N9 C26 C27 110.49(18) . . ?
N9 C26 H26A 109.6 . . ?
C27 C26 H26A 109.6 . . ?
N9 C26 H26B 109.6 . . ?
C27 C26 H26B 109.6 . . ?
H26A C26 H26B 108.1 . . ?
C8 C9 C10 108.70(19) . . ?
C8 C9 H9A 109.9 . . ?
C10 C9 H9A 109.9 . . ?
C8 C9 H9B 109.9 . . ?
C10 C9 H9B 109.9 . . ?
H9A C9 H9B 108.3 . . ?
N8 C24 H24A 109.5 . . ?
N8 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
N8 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N4 C12 H12A 109.5 . . ?
N4 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N4 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C26 C27 C28 108.13(19) . . ?
C26 C27 H27A 110.1 . . ?
C28 C27 H27A 110.1 . . ?
C26 C27 H27B 110.1 . . ?
C28 C27 H27B 110.1 . . ?
H27A C27 H27B 108.4 . . ?
N3 C11 H11A 109.5 . . ?
N3 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N3 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N7 C23 H23A 109.5 . . ?
N7 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
N7 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N2 C6 H6A 109.5 . . ?
N2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N2 C4 C3 -30.0(3) . . . . ?
C6 N2 C4 C3 160.9(2) . . . . ?
Mg1 O1 C1 N2 -79.8(6) . . . . ?
Mg1 O1 C1 N1 99.1(6) . . . . ?
C6 N2 C1 O1 -6.7(3) . . . . ?
C4 N2 C1 O1 -175.3(2) . . . . ?
C6 N2 C1 N1 174.4(2) . . . . ?
C4 N2 C1 N1 5.8(3) . . . . ?
C5 N1 C1 O1 11.4(3) . . . . ?
C2 N1 C1 O1 174.6(2) . . . . ?
C5 N1 C1 N2 -169.6(2) . . . . ?
C2 N1 C1 N2 -6.5(3) . . . . ?
Mg1 O4 C19 N7 -127.6(3) . . . . ?
Mg1 O4 C19 N8 52.6(4) . . . . ?
C24 N8 C19 O4 8.7(3) . . . . ?
C22 N8 C19 O4 178.7(2) . . . . ?
C24 N8 C19 N7 -171.16(19) . . . . ?
C22 N8 C19 N7 -1.1(3) . . . . ?
C13 N6 C16 C15 -27.4(3) . . . . ?
C18 N6 C16 C15 165.83(18) . . . . ?
Mg1 O3 C13 N5 63.6(3) . . . . ?
Mg1 O3 C13 N6 -116.4(2) . . . . ?
C17 N5 C13 O3 7.8(3) . . . . ?
C14 N5 C13 O3 170.09(18) . . . . ?
C17 N5 C13 N6 -172.20(18) . . . . ?
C14 N5 C13 N6 -9.9(3) . . . . ?
C18 N6 C13 O3 -7.7(3) . . . . ?
C16 N6 C13 O3 -173.81(18) . . . . ?
C18 N6 C13 N5 172.29(18) . . . . ?
C16 N6 C13 N5 6.1(3) . . . . ?
O4 C19 N7 C23 0.4(3) . . . . ?
N8 C19 N7 C23 -179.73(19) . . . . ?
O4 C19 N7 C20 -170.84(19) . . . . ?
N8 C19 N7 C20 9.0(3) . . . . ?
Mg1 O5 C25 N9 -75.4(4) . . . . ?
Mg1 O5 C25 N10 102.5(4) . . . . ?
C29 N9 C25 O5 -18.4(3) . . . . ?
C26 N9 C25 O5 -174.42(19) . . . . ?
C29 N9 C25 N10 163.70(19) . . . . ?
C26 N9 C25 N10 7.7(3) . . . . ?
C30 N10 C25 O5 4.9(3) . . . . ?
C28 N10 C25 O5 170.8(2) . . . . ?
C30 N10 C25 N9 -177.12(19) . . . . ?
C28 N10 C25 N9 -11.2(3) . . . . ?
Mg1 O2 C7 N4 86.3(3) . . . . ?
Mg1 O2 C7 N3 -95.3(3) . . . . ?
C12 N4 C7 O2 -2.1(3) . . . . ?
C10 N4 C7 O2 177.5(2) . . . . ?
C12 N4 C7 N3 179.4(2) . . . . ?
C10 N4 C7 N3 -1.0(3) . . . . ?
C11 N3 C7 O2 0.8(3) . . . . ?
C8 N3 C7 O2 173.0(2) . . . . ?
C11 N3 C7 N4 179.3(2) . . . . ?
C8 N3 C7 N4 -8.6(3) . . . . ?
C25 N10 C28 C27 36.7(3) . . . . ?
C30 N10 C28 C27 -157.2(2) . . . . ?
N6 C16 C15 C14 50.2(2) . . . . ?
C7 N3 C8 C9 38.3(3) . . . . ?
C11 N3 C8 C9 -149.3(2) . . . . ?
C19 N7 C20 C21 -37.1(3) . . . . ?
C23 N7 C20 C21 151.3(2) . . . . ?
C22 C21 C20 N7 55.4(3) . . . . ?
C1 N1 C2 C3 31.1(3) . . . . ?
C5 N1 C2 C3 -164.93(19) . . . . ?
C13 N5 C14 C15 34.3(3) . . . . ?
C17 N5 C14 C15 -162.55(18) . . . . ?
C16 C15 C14 N5 -53.5(2) . . . . ?
C7 N4 C10 C9 -20.5(3) . . . . ?
C12 N4 C10 C9 159.2(2) . . . . ?
N1 C2 C3 C4 -52.7(2) . . . . ?
N2 C4 C3 C2 52.4(2) . . . . ?
C19 N8 C22 C21 22.4(3) . . . . ?
C24 N8 C22 C21 -167.0(2) . . . . ?
C20 C21 C22 N8 -48.7(3) . . . . ?
C25 N9 C26 C27 -30.2(3) . . . . ?
C29 N9 C26 C27 172.98(19) . . . . ?
N3 C8 C9 C10 -56.4(3) . . . . ?
N4 C10 C9 C8 48.2(3) . . . . ?
N9 C26 C27 C28 53.4(3) . . . . ?
N10 C28 C27 C26 -56.4(2) . . . . ?

_refine_diff_density_max         1.227
_refine_diff_density_min         -0.590
_refine_diff_density_rms         0.069

####################################################################### 
# 
# 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_Pr_dmpu6_I7
_database_code_depnum_ccdc_archive 'CCDC 2209377'
loop_
_audit_author_name
_audit_author_address
'Lars Eriksson'
;Stockholm University
Sweden
;
_audit_update_record             
;
2022-09-25 deposited with the CCDC.	2023-12-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H72 N12 O6 Pr, I, 2(I3)'
_chemical_formula_sum            'C36 H72 I7 N12 O6 Pr'
_chemical_formula_weight         1798.26

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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_H-M_alt        'P -3'
_space_group_name_Hall           '-P 3'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'

_cell_length_a                   11.6236(18)
_cell_length_b                   11.6236(18)
_cell_length_c                   12.2134(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1429.1(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3001
_cell_measurement_theta_min      3.8701
_cell_measurement_theta_max      32.2976

_exptl_crystal_description       octahedron
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.090
_exptl_crystal_F_000             850
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.020
_exptl_crystal_size_mid          0.015
_exptl_crystal_size_min          0.012
_exptl_absorpt_coefficient_mu    4.681
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.855
_exptl_absorpt_correction_T_max  0.869
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET)
(compiled Apr 21 2008,18:23:10)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  
'Excalibur-III κ diffractometer with Sapphire-3 CCD'
_diffrn_measurement_method       'ω scans at different φ'
_diffrn_detector_area_resol_mean 16.5467
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        .
_diffrn_reflns_number            11630
_diffrn_reflns_av_unetI/netI     0.0992
_diffrn_reflns_av_R_equivalents  0.0561
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.883
_diffrn_reflns_theta_max         28.269
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             2370
_reflns_number_gt                1328
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;

_computing_structure_solution    'SHELXS (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0150P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.00131(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2370
_refine_ls_number_parameters     98
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0241
_refine_ls_wR_factor_ref         0.0412
_refine_ls_wR_factor_gt          0.0398
_refine_ls_goodness_of_fit_ref   0.703
_refine_ls_restrained_S_all      0.703
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pr1 Pr 0.000000 0.000000 0.000000 0.01241(13) Uani 1 6 d S T P . .
I1 I 0.000000 0.000000 0.500000 0.0361(2) Uani 1 6 d S T P . .
I21 I 0.333333 0.666667 0.58379(4) 0.02731(15) Uani 1 3 d S T P . .
I22 I 0.333333 0.666667 1.06001(4) 0.02739(15) Uani 1 3 d S T P . .
I23 I 0.333333 0.666667 0.82288(4) 0.01946(12) Uani 1 3 d S T P . .
O1 O 0.0935(2) -0.0975(2) 0.11004(18) 0.0164(6) Uani 1 1 d . . . . .
C1 C 0.1620(4) -0.1092(3) 0.1852(3) 0.0169(9) Uani 1 1 d . . . . .
N11 N 0.1027(3) -0.1878(3) 0.2715(2) 0.0185(7) Uani 1 1 d . . . . .
N12 N 0.2954(3) -0.0442(3) 0.1772(2) 0.0164(7) Uani 1 1 d . . . . .
C11 C -0.0426(3) -0.2645(4) 0.2790(3) 0.0266(10) Uani 1 1 d . . . . .
H11A H -0.074176 -0.215304 0.323014 0.040 Uiso 1 1 calc R U . . .
H11B H -0.069739 -0.350367 0.313750 0.040 Uiso 1 1 calc R U . . .
H11C H -0.080877 -0.279095 0.205414 0.040 Uiso 1 1 calc R U . . .
C12 C 0.3558(3) 0.0210(4) 0.0743(3) 0.0221(9) Uani 1 1 d . . . . .
H12A H 0.303309 -0.035391 0.013144 0.033 Uiso 1 1 calc R U . . .
H12B H 0.446440 0.035719 0.070172 0.033 Uiso 1 1 calc R U . . .
H12C H 0.358556 0.106506 0.070312 0.033 Uiso 1 1 calc R U . . .
C13 C 0.1771(4) -0.1958(4) 0.3650(3) 0.0268(10) Uani 1 1 d . . . . .
H13A H 0.187473 -0.274908 0.357235 0.032 Uiso 1 1 calc R U . . .
H13B H 0.127199 -0.205594 0.433363 0.032 Uiso 1 1 calc R U . . .
C14 C 0.3106(4) -0.0741(4) 0.3719(3) 0.0217(9) Uani 1 1 d . . . . .
H14A H 0.364383 -0.086213 0.428690 0.026 Uiso 1 1 calc R U . . .
H14B H 0.300835 0.002795 0.392905 0.026 Uiso 1 1 calc R U . . .
C15 C 0.3801(4) -0.0476(4) 0.2630(3) 0.0243(10) Uani 1 1 d . . . . .
H15A H 0.464265 0.038459 0.265557 0.029 Uiso 1 1 calc R U . . .
H15B H 0.401644 -0.118194 0.246962 0.029 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pr1 O1 2.346(2) . ?
Pr1 O1 2.346(2) 5 ?
Pr1 O1 2.346(2) 2 ?
Pr1 O1 2.346(2) 4 ?
Pr1 O1 2.346(2) 6 ?
Pr1 O1 2.346(2) 3 ?
I21 I23 2.9202(7) . ?
I22 I23 2.8961(7) . ?
O1 C1 1.266(4) . ?
C1 N11 1.339(4) . ?
C1 N12 1.346(4) . ?
N11 C13 1.463(4) . ?
N11 C11 1.466(4) . ?
N12 C15 1.452(4) . ?
N12 C12 1.454(4) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.490(5) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.506(5) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Pr1 O1 89.56(8) . 5 ?
O1 Pr1 O1 90.44(8) . 2 ?
O1 Pr1 O1 180.00(14) 5 2 ?
O1 Pr1 O1 180.0 . 4 ?
O1 Pr1 O1 90.44(8) 5 4 ?
O1 Pr1 O1 89.56(8) 2 4 ?
O1 Pr1 O1 89.56(8) . 6 ?
O1 Pr1 O1 90.44(8) 5 6 ?
O1 Pr1 O1 89.56(8) 2 6 ?
O1 Pr1 O1 90.44(8) 4 6 ?
O1 Pr1 O1 90.44(8) . 3 ?
O1 Pr1 O1 89.56(8) 5 3 ?
O1 Pr1 O1 90.44(8) 2 3 ?
O1 Pr1 O1 89.56(8) 4 3 ?
O1 Pr1 O1 180.0(2) 6 3 ?
I22 I23 I21 180.0 . . ?
C1 O1 Pr1 159.2(2) . . ?
O1 C1 N11 120.5(3) . . ?
O1 C1 N12 119.8(3) . . ?
N11 C1 N12 119.7(3) . . ?
C1 N11 C13 122.7(3) . . ?
C1 N11 C11 120.5(3) . . ?
C13 N11 C11 116.7(3) . . ?
C1 N12 C15 122.6(3) . . ?
C1 N12 C12 118.4(3) . . ?
C15 N12 C12 118.7(3) . . ?
N11 C11 H11A 109.5 . . ?
N11 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N11 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N12 C12 H12A 109.5 . . ?
N12 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N12 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N11 C13 C14 110.6(3) . . ?
N11 C13 H13A 109.5 . . ?
C14 C13 H13A 109.5 . . ?
N11 C13 H13B 109.5 . . ?
C14 C13 H13B 109.5 . . ?
H13A C13 H13B 108.1 . . ?
C13 C14 C15 110.0(3) . . ?
C13 C14 H14A 109.7 . . ?
C15 C14 H14A 109.7 . . ?
C13 C14 H14B 109.7 . . ?
C15 C14 H14B 109.7 . . ?
H14A C14 H14B 108.2 . . ?
N12 C15 C14 109.9(3) . . ?
N12 C15 H15A 109.7 . . ?
C14 C15 H15A 109.7 . . ?
N12 C15 H15B 109.7 . . ?
C14 C15 H15B 109.7 . . ?
H15A C15 H15B 108.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Pr1 O1 C1 N11 109.5(6) . . . . ?
Pr1 O1 C1 N12 -71.8(7) . . . . ?
O1 C1 N11 C13 -174.5(3) . . . . ?
N12 C1 N11 C13 6.8(5) . . . . ?
O1 C1 N11 C11 1.7(5) . . . . ?
N12 C1 N11 C11 -177.0(3) . . . . ?
O1 C1 N12 C15 176.7(3) . . . . ?
N11 C1 N12 C15 -4.6(5) . . . . ?
O1 C1 N12 C12 -9.6(5) . . . . ?
N11 C1 N12 C12 169.1(3) . . . . ?
C1 N11 C13 C14 22.3(5) . . . . ?
C11 N11 C13 C14 -154.1(3) . . . . ?
N11 C13 C14 C15 -51.4(4) . . . . ?
C1 N12 C15 C14 -26.0(5) . . . . ?
C12 N12 C15 C14 160.3(3) . . . . ?
C13 C14 C15 N12 53.1(4) . . . . ?

_refine_diff_density_max         0.616
_refine_diff_density_min         -0.647
_refine_diff_density_rms         0.114

####################################################################### 
# 
# 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_Ca_dmpu6_I2
_database_code_depnum_ccdc_archive 'CCDC 2206128'
loop_
_audit_author_name
_audit_author_address
'Lars Eriksson'
;Stockholm University
Sweden
;
_audit_update_record             
;
2022-09-08 deposited with the CCDC.	2023-12-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H72 Ca N12 O6, 2(I)'
_chemical_formula_sum            'C36 H72 Ca I2 N12 O6'
_chemical_formula_weight         1062.93

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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_H-M_alt        'P -3'
_space_group_name_Hall           '-P 3'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'

_cell_length_a                   12.9549(18)
_cell_length_b                   12.9549(18)
_cell_length_c                   8.5602(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1244.2(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2024
_cell_measurement_theta_min      3.70
_cell_measurement_theta_max      21.5

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_F_000             546
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    1.418
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.45
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Incotec 1MyS'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       'ω scans and φ scans'
_diffrn_detector_area_resol_mean 0.1
_diffrn_reflns_number            7894
_diffrn_reflns_av_unetI/netI     0.0097
_diffrn_reflns_av_R_equivalents  0.0164
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.993
_diffrn_reflns_theta_max         23.536
_diffrn_reflns_theta_full        23.536
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             1246
_reflns_number_gt                1100
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _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       'APEX3 (Bruker, 2020)'
_computing_cell_refinement       'APEX3 (Bruker, 2020)'
_computing_data_reduction        'APEX3 (Bruker, 2020)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0545P)²+1.7945P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.0043(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1246
_refine_ls_number_parameters     90
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0547
_refine_ls_R_factor_gt           0.0494
_refine_ls_wR_factor_ref         0.1338
_refine_ls_wR_factor_gt          0.1299
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_restrained_S_all      1.081
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.666667 0.333333 0.21996(15) 0.1436(6) Uani 1 3 d S T P . .
Ca1 Ca 1.000000 0.000000 0.500000 0.0371(4) Uani 1 6 d S T P . .
O1 O 0.8337(2) -0.0562(2) 0.3443(3) 0.0534(7) Uani 1 1 d . . . . .
C1 C 0.7398(3) -0.0666(3) 0.2897(4) 0.0461(9) Uani 1 1 d . . . . .
N11 N 0.6336(3) -0.1591(3) 0.3287(4) 0.0658(10) Uani 1 1 d . . . . .
N12 N 0.7420(3) 0.0139(3) 0.1908(4) 0.0622(9) Uani 1 1 d . . . . .
C11 C 0.6286(5) -0.2484(5) 0.4347(8) 0.114(2) Uani 1 1 d . . . . .
H11A H 0.658688 -0.293851 0.383223 0.170 Uiso 1 1 calc R U . . .
H11B H 0.547523 -0.300537 0.465897 0.170 Uiso 1 1 calc R U . . .
H11C H 0.676268 -0.210162 0.525205 0.170 Uiso 1 1 calc R U . . .
C12 C 0.8549(5) 0.1130(6) 0.1410(7) 0.107(2) Uani 1 1 d . . . . .
H12A H 0.917432 0.095851 0.162890 0.160 Uiso 1 1 calc R U . . .
H12B H 0.869824 0.183669 0.196181 0.160 Uiso 1 1 calc R U . . .
H12C H 0.852292 0.125242 0.030767 0.160 Uiso 1 1 calc R U . . .
C13 C 0.5215(4) -0.1750(6) 0.2718(8) 0.103(2) Uani 1 1 d . . . . .
H13A H 0.494065 -0.231224 0.185779 0.124 Uiso 1 1 calc R U . . .
H13B H 0.462590 -0.208599 0.354541 0.124 Uiso 1 1 calc R U . . .
C14 C 0.5308(5) -0.0658(7) 0.2204(10) 0.121(2) Uani 1 1 d . . . . .
H14A H 0.532916 -0.020036 0.311249 0.145 Uiso 1 1 calc R U . . .
H14B H 0.459978 -0.083934 0.160924 0.145 Uiso 1 1 calc R U . . .
C15 C 0.6353(5) 0.0073(5) 0.1246(6) 0.0827(15) Uani 1 1 d . . . . .
H15A H 0.646683 0.087045 0.116263 0.099 Uiso 1 1 calc R U . . .
H15B H 0.622379 -0.026141 0.020272 0.099 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ca1 O1 2.319(2) 4_756 ?
Ca1 O1 2.319(2) 5_666 ?
Ca1 O1 2.319(2) 2_645 ?
Ca1 O1 2.319(2) 6_546 ?
Ca1 O1 2.319(2) 3_765 ?
Ca1 O1 2.319(2) . ?
O1 C1 1.246(4) . ?
C1 N12 1.333(5) . ?
C1 N11 1.338(5) . ?
N11 C13 1.446(5) . ?
N11 C11 1.446(6) . ?
N12 C12 1.446(6) . ?
N12 C15 1.456(6) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 C14 1.428(9) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 C15 1.456(8) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ca1 O1 90.27(9) 4_756 5_666 ?
O1 Ca1 O1 89.73(9) 4_756 2_645 ?
O1 Ca1 O1 180.0 5_666 2_645 ?
O1 Ca1 O1 90.27(9) 4_756 6_546 ?
O1 Ca1 O1 90.27(9) 5_666 6_546 ?
O1 Ca1 O1 89.73(9) 2_645 6_546 ?
O1 Ca1 O1 89.73(9) 4_756 3_765 ?
O1 Ca1 O1 89.73(9) 5_666 3_765 ?
O1 Ca1 O1 90.27(9) 2_645 3_765 ?
O1 Ca1 O1 180.00(11) 6_546 3_765 ?
O1 Ca1 O1 180.0 4_756 . ?
O1 Ca1 O1 89.72(9) 5_666 . ?
O1 Ca1 O1 90.28(9) 2_645 . ?
O1 Ca1 O1 89.72(9) 6_546 . ?
O1 Ca1 O1 90.28(9) 3_765 . ?
C1 O1 Ca1 162.4(2) . . ?
O1 C1 N12 121.1(3) . . ?
O1 C1 N11 121.0(3) . . ?
N12 C1 N11 117.9(3) . . ?
C1 N11 C13 123.6(4) . . ?
C1 N11 C11 119.2(3) . . ?
C13 N11 C11 117.2(4) . . ?
C1 N12 C12 119.9(4) . . ?
C1 N12 C15 123.6(4) . . ?
C12 N12 C15 116.5(4) . . ?
N11 C11 H11A 109.5 . . ?
N11 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N11 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N12 C12 H12A 109.5 . . ?
N12 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N12 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 N11 112.4(5) . . ?
C14 C13 H13A 109.1 . . ?
N11 C13 H13A 109.1 . . ?
C14 C13 H13B 109.1 . . ?
N11 C13 H13B 109.1 . . ?
H13A C13 H13B 107.9 . . ?
C13 C14 C15 114.1(5) . . ?
C13 C14 H14A 108.7 . . ?
C15 C14 H14A 108.7 . . ?
C13 C14 H14B 108.7 . . ?
C15 C14 H14B 108.7 . . ?
H14A C14 H14B 107.6 . . ?
C14 C15 N12 111.4(4) . . ?
C14 C15 H15A 109.3 . . ?
N12 C15 H15A 109.3 . . ?
C14 C15 H15B 109.3 . . ?
N12 C15 H15B 109.3 . . ?
H15A C15 H15B 108.0 . . ?

_refine_diff_density_max         0.714
_refine_diff_density_min         -0.557
_refine_diff_density_rms         0.055

####################################################################### 
# 
# 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_r
_database_code_depnum_ccdc_archive 'CCDC 2297621'
loop_
_audit_author_name
_audit_author_address
'Lars Eriksson'
;Stockholm University
Sweden
;
_audit_update_record             
;
2023-11-18 deposited with the CCDC.	2023-12-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H72 Ca F6 N12 O12 S2'
_chemical_formula_weight         1107.27

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_H-M_alt        'P -3'
_space_group_name_Hall           '-P 3'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'

_cell_length_a                   13.532(2)
_cell_length_b                   13.532(2)
_cell_length_c                   8.7287(14)
_cell_angle_alpha                90.000(3)
_cell_angle_beta                 90.000(3)
_cell_angle_gamma                120.000(3)
_cell_volume                     1384.3(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    999?
_cell_measurement_theta_min      2.0
_cell_measurement_theta_max      24.9

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_F_000             586
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.17
_exptl_absorpt_coefficient_mu    0.272
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'Bruker SADABS (1998)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker SMART CCD diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7993
_diffrn_reflns_av_unetI/netI     0.1046
_diffrn_reflns_av_R_equivalents  0.1043
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         1.738
_diffrn_reflns_theta_max         25.657
_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             1768
_reflns_number_gt                713
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _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 SMART (1998b)'
_computing_cell_refinement       '(Bruker SMART and SAINT (1998b)'
_computing_data_reduction        '(Bruker SAINT (1998b)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.1290P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       .
_refine_ls_extinction_expression ?
_refine_ls_number_reflns         1768
_refine_ls_number_parameters     105
_refine_ls_number_restraints     27
_refine_ls_R_factor_all          0.2370
_refine_ls_R_factor_gt           0.1299
_refine_ls_wR_factor_ref         0.3683
_refine_ls_wR_factor_gt          0.3313
_refine_ls_goodness_of_fit_ref   1.463
_refine_ls_restrained_S_all      1.513
_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 0.000000 0.000000 0.000000 0.0520(12) Uani 1 6 d S T P . .
O1 O 0.0630(4) 0.1614(4) 0.1528(5) 0.0678(16) Uani 1 1 d . . . . .
C1 C 0.0800(6) 0.2516(6) 0.2120(7) 0.0571(18) Uiso 1 1 d . . . . .
N11 N 0.0034(5) 0.2554(5) 0.3034(7) 0.0738(19) Uani 1 1 d . . . . .
N12 N 0.1763(6) 0.3503(5) 0.1812(7) 0.081(2) Uani 1 1 d . . . . .
C11 C -0.0956(8) 0.1499(8) 0.3500(12) 0.117(4) Uani 1 1 d . . . . .
H11A H -0.142679 0.166259 0.415266 0.176 Uiso 1 1 calc R U . . .
H11B H -0.138277 0.109298 0.260967 0.176 Uiso 1 1 calc R U . . .
H11C H -0.071562 0.103942 0.404600 0.176 Uiso 1 1 calc R U . . .
C12 C 0.2670(8) 0.3482(7) 0.0933(12) 0.127(4) Uani 1 1 d . . . . .
H12A H 0.329452 0.424671 0.081104 0.191 Uiso 1 1 calc R U . . .
H12B H 0.292858 0.303299 0.146723 0.191 Uiso 1 1 calc R U . . .
H12C H 0.238383 0.315320 -0.005599 0.191 Uiso 1 1 calc R U . . .
C13 C 0.0153(8) 0.3582(8) 0.3741(10) 0.094(3) Uani 1 1 d . . . . .
H13A H 0.047335 0.366908 0.475874 0.113 Uiso 1 1 calc R U . . .
H13B H -0.059333 0.351256 0.384037 0.113 Uiso 1 1 calc R U . . .
C14 C 0.0890(11) 0.4585(9) 0.2824(13) 0.124(4) Uani 1 1 d . . . . .
H14A H 0.104912 0.527192 0.337466 0.148 Uiso 1 1 calc R U . . .
H14B H 0.051332 0.456571 0.186895 0.148 Uiso 1 1 calc R U . . .
C15 C 0.2005(10) 0.4592(7) 0.2493(11) 0.120(4) Uani 1 1 d . . . . .
H15A H 0.247018 0.521128 0.179620 0.144 Uiso 1 1 calc R U . . .
H15B H 0.242849 0.471732 0.343857 0.144 Uiso 1 1 calc R U . . .
S2 S 0.666667 0.333333 0.3485(11) 0.219(4) Uani 1 3 d DS TU P . .
O2 O 0.700(2) 0.2639(17) 0.408(2) 0.498(16) Uani 1 1 d D U . . .
C2 C 0.666667 0.333333 0.134(3) 0.319(17) Uani 1 3 d DS TU P . .
F2 F 0.7706(16) 0.3740(19) 0.104(2) 0.481(14) Uani 1 1 d D U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ca1 O1 2.327(4) 6 ?
Ca1 O1 2.327(4) 3 ?
Ca1 O1 2.327(4) . ?
Ca1 O1 2.327(4) 2 ?
Ca1 O1 2.327(4) 5 ?
Ca1 O1 2.327(4) 4 ?
O1 C1 1.236(8) . ?
C1 N11 1.329(9) . ?
C1 N12 1.347(9) . ?
N11 C11 1.444(10) . ?
N11 C13 1.455(9) . ?
N12 C12 1.459(10) . ?
N12 C15 1.467(10) . ?
C13 C14 1.458(13) . ?
C14 C15 1.532(13) . ?
S2 O2 1.331(12) . ?
S2 O2 1.331(12) 2_655 ?
S2 O2 1.331(12) 3_665 ?
S2 C2 1.87(2) . ?
C2 F2 1.256(17) . ?
C2 F2 1.256(17) 3_665 ?
C2 F2 1.256(17) 2_655 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ca1 O1 180.0(3) 6 3 ?
O1 Ca1 O1 89.60(16) 6 . ?
O1 Ca1 O1 90.40(16) 3 . ?
O1 Ca1 O1 89.60(16) 6 2 ?
O1 Ca1 O1 90.40(16) 3 2 ?
O1 Ca1 O1 90.40(16) . 2 ?
O1 Ca1 O1 90.40(16) 6 5 ?
O1 Ca1 O1 89.60(16) 3 5 ?
O1 Ca1 O1 89.60(16) . 5 ?
O1 Ca1 O1 180.0(4) 2 5 ?
O1 Ca1 O1 90.40(16) 6 4 ?
O1 Ca1 O1 89.60(16) 3 4 ?
O1 Ca1 O1 180.0 . 4 ?
O1 Ca1 O1 89.60(16) 2 4 ?
O1 Ca1 O1 90.40(16) 5 4 ?
C1 O1 Ca1 165.0(4) . . ?
O1 C1 N11 121.7(7) . . ?
O1 C1 N12 120.4(7) . . ?
N11 C1 N12 117.9(7) . . ?
C1 N11 C11 119.1(7) . . ?
C1 N11 C13 125.2(7) . . ?
C11 N11 C13 115.5(7) . . ?
C1 N12 C12 119.5(6) . . ?
C1 N12 C15 122.3(7) . . ?
C12 N12 C15 117.7(7) . . ?
N11 C13 C14 110.8(7) . . ?
C13 C14 C15 108.8(9) . . ?
N12 C15 C14 110.3(7) . . ?
O2 S2 O2 105.8(12) . 2_655 ?
O2 S2 O2 105.8(12) . 3_665 ?
O2 S2 O2 105.8(12) 2_655 3_665 ?
O2 S2 C2 113.0(10) . . ?
O2 S2 C2 113.0(10) 2_655 . ?
O2 S2 C2 113.0(10) 3_665 . ?
F2 C2 F2 115.7(10) . 3_665 ?
F2 C2 F2 115.7(10) . 2_655 ?
F2 C2 F2 115.7(10) 3_665 2_655 ?
F2 C2 S2 102.1(14) . . ?
F2 C2 S2 102.1(14) 3_665 . ?
F2 C2 S2 102.1(14) 2_655 . ?

_refine_diff_density_max         0.858
_refine_diff_density_min         -0.598
_refine_diff_density_rms         0.114

####################################################################### 
# 
# 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_ca_dmpu6_clo4_2
_database_code_depnum_ccdc_archive 'CCDC 2297623'
loop_
_audit_author_name
_audit_author_address
'Lars Eriksson'
;Stockholm University
Sweden
;
_audit_update_record             
;
2023-09-26 deposited with the CCDC.	2023-12-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
Hexakis(dimethylpropyleneurea)calcium(II)perchlorate
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H72 Ca Cl2 N12 O14'
_chemical_formula_weight         1008.04

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'

_symmetry_cell_setting           Hexagonal
_symmetry_space_group_name_H-M   P-3

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'

_cell_length_a                   13.083(3)
_cell_length_b                   13.083(3)
_cell_length_c                   8.553(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     1267.8(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    1270
_cell_measurement_theta_min      1.80
_cell_measurement_theta_max      27.47

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             538
_exptl_absorpt_coefficient_mu    0.299
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.8896
_exptl_absorpt_correction_T_max  0.9426
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART CCD diffractometer'
_diffrn_measurement_method       'Omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        
;
Neglible as determined from a repetition of the first
50 frames at the end of the experiment
;
_diffrn_reflns_number            9888
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_sigmaI/netI    0.0336
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         1.80
_diffrn_reflns_theta_max         27.47
_reflns_number_total             1914
_reflns_number_gt                1270
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART (1998)'
_computing_cell_refinement       'Bruker SMART and SAINT (1998)'
_computing_data_reduction        'Bruker SAINT (1998)'
_computing_structure_solution    'Bruker SHELXTL (1998)'
_computing_structure_refinement  'Bruker SHELXTL (1998)'
_computing_molecular_graphics    'Bruker SHELXTL (1998)'
_computing_publication_material  'Bruker SHELXTL (1998)'


_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)+(0.0900P)²+0.0000P] 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     SHELXL
_refine_ls_extinction_coef       0.021(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1914
_refine_ls_number_parameters     116
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0450
_refine_ls_wR_factor_ref         0.1348
_refine_ls_wR_factor_gt          0.1269
_refine_ls_goodness_of_fit_ref   0.916
_refine_ls_restrained_S_all      0.916
_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
Ca1 Ca 0.0000 0.0000 0.0000 0.0371(3) Uani 1 6 d S . .
O1 O 0.10765(11) 0.16565(10) 0.15653(15) 0.0527(4) Uani 1 1 d . . .
N1 N 0.26955(15) 0.25712(15) 0.3090(2) 0.0609(5) Uani 1 1 d . . .
N2 N 0.20174(16) 0.36425(14) 0.1741(2) 0.0628(5) Uani 1 1 d . . .
C1 C 0.18980(15) 0.25856(15) 0.21082(19) 0.0452(4) Uani 1 1 d . . .
C2 C 0.3688(2) 0.3628(2) 0.3746(3) 0.0786(7) Uani 1 1 d . . .
H2A H 0.4369 0.3520 0.3806 0.094 Uiso 1 1 calc R . .
H2B H 0.3494 0.3748 0.4800 0.094 Uiso 1 1 calc R . .
C3 C 0.3986(3) 0.4670(3) 0.2806(4) 0.1110(11) Uani 1 1 d . . .
H4A H 0.4510 0.5370 0.3403 0.133 Uiso 1 1 calc R . .
H4B H 0.4409 0.4659 0.1880 0.133 Uiso 1 1 calc R . .
C4 C 0.2966(3) 0.4750(2) 0.2327(4) 0.1006(10) Uani 1 1 d . . .
H3A H 0.2681 0.5000 0.3212 0.121 Uiso 1 1 calc R . .
H3B H 0.3200 0.5346 0.1519 0.121 Uiso 1 1 calc R . .
C5 C 0.2562(3) 0.1450(3) 0.3571(4) 0.0975(9) Uani 1 1 d . . .
H5A H 0.2593 0.1425 0.4691 0.146 Uiso 1 1 calc R . .
H5B H 0.3187 0.1361 0.3131 0.146 Uiso 1 1 calc R . .
H5C H 0.1815 0.0821 0.3211 0.146 Uiso 1 1 calc R . .
C6 C 0.1162(3) 0.3689(2) 0.0726(4) 0.1026(11) Uani 1 1 d . . .
H6A H 0.1356 0.4495 0.0594 0.154 Uiso 1 1 calc R . .
H6B H 0.0391 0.3245 0.1182 0.154 Uiso 1 1 calc R . .
H6C H 0.1169 0.3359 -0.0273 0.154 Uiso 1 1 calc R . .
Cl1 Cl -0.3333 0.3333 0.26775(18) 0.0893(4) Uani 1 3 d S . .
O3A O -0.3342(8) 0.4325(9) 0.3225(18) 0.184(9) Uani 0.49(2) 1 d P . .
O3B O -0.3500(10) 0.4182(10) 0.2007(16) 0.184(7) Uani 0.51(2) 1 d P . .
O4A O -0.3333 0.3333 0.1166(18) 0.229(12) Uani 0.49(2) 3 d SP . .
O4B O -0.3333 0.3333 0.4177(13) 0.240(12) Uani 0.51(2) 3 d SP . .


_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 O1 2.3282(12) 4 ?
Ca1 O1 2.3282(12) . ?
Ca1 O1 2.3282(12) 6 ?
Ca1 O1 2.3282(12) 2 ?
Ca1 O1 2.3282(12) 5 ?
Ca1 O1 2.3282(12) 3 ?
O1 C1 1.242(2) . ?
N1 C1 1.347(2) . ?
N1 C5 1.447(3) . ?
N1 C2 1.455(3) . ?
N2 C1 1.349(2) . ?
N2 C6 1.441(3) . ?
N2 C4 1.446(3) . ?
C2 C3 1.459(4) . ?
C3 C4 1.448(4) . ?
Cl1 O4B 1.282(11) . ?
Cl1 O4A 1.293(15) . ?
Cl1 O3B 1.361(8) 3_455 ?
Cl1 O3B 1.361(8) 2_565 ?
Cl1 O3B 1.361(8) . ?
Cl1 O3A 1.385(7) 3_455 ?
Cl1 O3A 1.385(7) 2_565 ?
Cl1 O3A 1.385(7) . ?
O3A O3B 1.061(11) . ?
O3A O4B 1.536(16) . ?
O3B O4A 1.429(16) . ?
O4A O3B 1.429(16) 3_455 ?
O4A O3B 1.429(16) 2_565 ?
O4B O3A 1.536(16) 3_455 ?
O4B O3A 1.536(16) 2_565 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ca1 O1 180.00(8) 4 . ?
O1 Ca1 O1 90.23(5) 4 6 ?
O1 Ca1 O1 89.77(5) . 6 ?
O1 Ca1 O1 89.77(5) 4 2 ?
O1 Ca1 O1 90.23(5) . 2 ?
O1 Ca1 O1 89.77(5) 6 2 ?
O1 Ca1 O1 90.23(5) 4 5 ?
O1 Ca1 O1 89.77(5) . 5 ?
O1 Ca1 O1 90.23(5) 6 5 ?
O1 Ca1 O1 180.0 2 5 ?
O1 Ca1 O1 89.77(5) 4 3 ?
O1 Ca1 O1 90.23(5) . 3 ?
O1 Ca1 O1 180.00(7) 6 3 ?
O1 Ca1 O1 90.23(5) 2 3 ?
O1 Ca1 O1 89.77(5) 5 3 ?
C1 O1 Ca1 161.97(12) . . ?
C1 N1 C5 119.30(18) . . ?
C1 N1 C2 123.84(18) . . ?
C5 N1 C2 116.84(19) . . ?
C1 N2 C6 119.31(17) . . ?
C1 N2 C4 123.21(18) . . ?
C6 N2 C4 117.48(19) . . ?
O1 C1 N1 121.12(17) . . ?
O1 C1 N2 121.08(17) . . ?
N1 C1 N2 117.79(16) . . ?
N1 C2 C3 111.7(2) . . ?
C4 C3 C2 113.5(3) . . ?
N2 C4 C3 112.7(2) . . ?
O4B Cl1 O4A 180.000(5) . . ?
O4B Cl1 O3B 114.9(7) . 3_455 ?
O4A Cl1 O3B 65.1(7) . 3_455 ?
O4B Cl1 O3B 114.9(7) . 2_565 ?
O4A Cl1 O3B 65.1(7) . 2_565 ?
O3B Cl1 O3B 103.5(8) 3_455 2_565 ?
O4B Cl1 O3B 114.9(7) . . ?
O4A Cl1 O3B 65.1(7) . . ?
O3B Cl1 O3B 103.5(8) 3_455 . ?
O3B Cl1 O3B 103.5(8) 2_565 . ?
O4B Cl1 O3A 70.2(7) . 3_455 ?
O4A Cl1 O3A 109.8(7) . 3_455 ?
O3B Cl1 O3A 45.4(5) 3_455 3_455 ?
O3B Cl1 O3A 117.2(8) 2_565 3_455 ?
O3B Cl1 O3A 132.2(7) . 3_455 ?
O4B Cl1 O3A 70.2(7) . 2_565 ?
O4A Cl1 O3A 109.8(7) . 2_565 ?
O3B Cl1 O3A 132.2(7) 3_455 2_565 ?
O3B Cl1 O3A 45.4(5) 2_565 2_565 ?
O3B Cl1 O3A 117.2(8) . 2_565 ?
O3A Cl1 O3A 109.2(7) 3_455 2_565 ?
O4B Cl1 O3A 70.2(7) . . ?
O4A Cl1 O3A 109.8(7) . . ?
O3B Cl1 O3A 117.2(8) 3_455 . ?
O3B Cl1 O3A 132.2(7) 2_565 . ?
O3B Cl1 O3A 45.4(5) . . ?
O3A Cl1 O3A 109.2(7) 3_455 . ?
O3A Cl1 O3A 109.2(7) 2_565 . ?
O3B O3A Cl1 66.1(6) . . ?
O3B O3A O4B 117.1(11) . . ?
Cl1 O3A O4B 51.8(6) . . ?
O3A O3B Cl1 68.5(8) . . ?
O3A O3B O4A 122.6(13) . . ?
Cl1 O3B O4A 55.2(7) . . ?
Cl1 O4A O3B 59.8(7) . 3_455 ?
Cl1 O4A O3B 59.8(7) . 2_565 ?
O3B O4A O3B 96.9(9) 3_455 2_565 ?
Cl1 O4A O3B 59.8(7) . . ?
O3B O4A O3B 96.9(9) 3_455 . ?
O3B O4A O3B 96.9(9) 2_565 . ?
Cl1 O4B O3A 58.0(5) . 3_455 ?
Cl1 O4B O3A 58.0(5) . 2_565 ?
O3A O4B O3A 94.5(7) 3_455 2_565 ?
Cl1 O4B O3A 58.0(5) . . ?
O3A O4B O3A 94.5(7) 3_455 . ?
O3A O4B O3A 94.5(7) 2_565 . ?

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        27.47
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         0.459
_refine_diff_density_min         -0.254
_refine_diff_density_rms         0.041
####################################################################### 
# 
# 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_r_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2249335'
loop_
_audit_author_name
_audit_author_address
'Lars Eriksson'
;Stockholm University
Sweden
;
_audit_update_record             
;
2023-11-18 deposited with the CCDC.	2023-12-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C46 H72 Ba F6 N12 O12 S2'
_chemical_formula_weight         1300.61

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_H-M_alt        'P -3'
_space_group_name_Hall           '-P 3'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'

_cell_length_a                   13.9909(3)
_cell_length_b                   13.9909(3)
_cell_length_c                   8.4390(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1430.58(8)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    999
_cell_measurement_theta_min      2.5
_cell_measurement_theta_max      25.1

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_F_000             670
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_exptl_absorpt_coefficient_mu    0.854
_shelx_estimated_absorpt_T_min   .
_shelx_estimated_absorpt_T_max   .
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6121
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker SMART CCD diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9903
_diffrn_reflns_av_unetI/netI     0.0157
_diffrn_reflns_av_R_equivalents  0.0233
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.413
_diffrn_reflns_theta_max         25.674
_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 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1811
_reflns_number_gt                1798
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.1115P)²] 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_number_reflns         1811
_refine_ls_number_parameters     122
_refine_ls_number_restraints     117
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0534
_refine_ls_wR_factor_ref         0.1429
_refine_ls_wR_factor_gt          0.1424
_refine_ls_goodness_of_fit_ref   1.206
_refine_ls_restrained_S_all      1.216
_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
Ba1 Ba 0.000000 0.000000 0.000000 0.0505(2) Uani 1 6 d S TU P . .
O1 O 0.1770(3) 0.1060(3) 0.1752(4) 0.0762(8) Uani 1 1 d . U . . .
C1 C 0.2661(3) 0.1820(4) 0.2238(4) 0.0613(9) Uani 1 1 d . U . . .
N11 N 0.3615(3) 0.1843(4) 0.1880(5) 0.0828(11) Uani 1 1 d . U . . .
N12 N 0.2705(4) 0.2627(4) 0.3133(5) 0.0757(10) Uani 1 1 d . U . . .
C11 C 0.3573(6) 0.0929(8) 0.0998(11) 0.133(3) Uani 1 1 d . U . . .
H11A H 0.281726 0.037135 0.083089 0.199 Uiso 1 1 calc R U . . .
H11B H 0.394216 0.062190 0.158912 0.199 Uiso 1 1 calc R U . . .
H11C H 0.393191 0.119030 -0.000668 0.199 Uiso 1 1 calc R U . . .
C12 C 0.1701(6) 0.2548(7) 0.3674(10) 0.114(2) Uani 1 1 d . U . . .
H12A H 0.119465 0.180070 0.398205 0.171 Uiso 1 1 calc R U . . .
H12B H 0.138171 0.276127 0.283642 0.171 Uiso 1 1 calc R U . . .
H12C H 0.185154 0.302782 0.456647 0.171 Uiso 1 1 calc R U . . .
C13 C 0.4684(5) 0.2693(7) 0.2494(9) 0.115(2) Uani 1 1 d . U . . .
H13A H 0.525689 0.283832 0.172574 0.138 Uiso 1 1 calc R U . . .
H13B H 0.485330 0.243297 0.346184 0.138 Uiso 1 1 calc R U . . .
C14 C 0.4667(6) 0.3727(6) 0.2822(12) 0.125(2) Uani 1 1 d . U . . .
H14A H 0.534600 0.425205 0.334697 0.150 Uiso 1 1 calc R U . . .
H14B H 0.461828 0.405204 0.183107 0.150 Uiso 1 1 calc R U . . .
C15 C 0.3734(6) 0.3504(5) 0.3817(9) 0.1001(17) Uani 1 1 d . U . . .
H15A H 0.368854 0.417026 0.392825 0.120 Uiso 1 1 calc R U . . .
H15B H 0.383841 0.328360 0.486317 0.120 Uiso 1 1 calc R U . . .
O101 O 0.7140(17) 0.4404(14) 0.636(2) 0.462(16) Uani 1 1 d D U . A 2
S102 S 0.6216(9) 0.3424(9) 0.7057(19) 0.220(7) Uani 0.3333 1 d D U P A 2
C103 C 0.6858(18) 0.314(4) 0.873(5) 0.32(3) Uani 0.3333 1 d D U P A 2
F104 F 0.7920(13) 0.392(2) 0.872(2) 0.466(14) Uani 1 1 d D U . A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ba1 O1 2.616(3) 4 ?
Ba1 O1 2.616(3) 5 ?
Ba1 O1 2.616(3) 2 ?
Ba1 O1 2.616(3) 6 ?
Ba1 O1 2.616(3) 3 ?
Ba1 O1 2.616(3) . ?
O1 C1 1.235(5) . ?
C1 N12 1.334(6) . ?
C1 N11 1.353(6) . ?
N11 C11 1.456(9) . ?
N11 C13 1.464(7) . ?
N12 C12 1.427(8) . ?
N12 C15 1.464(7) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 C14 1.485(12) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 C15 1.448(12) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
O101 S102 1.094(15) 3_665 ?
O101 S102 1.459(9) . ?
O101 S102 2.069(16) 2_655 ?
S102 S102 1.22(2) 3_665 ?
S102 S102 1.22(2) 2_655 ?
S102 C103 1.48(5) 3_665 ?
S102 C103 1.61(2) 2_655 ?
S102 F104 1.671(19) 2_655 ?
S102 C103 1.819(9) . ?
C103 C103 0.80(9) 2_655 ?
C103 C103 0.80(9) 3_665 ?
C103 F104 1.333(10) . ?
C103 F104 1.37(4) 3_665 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ba1 O1 91.21(11) 4 5 ?
O1 Ba1 O1 88.79(11) 4 2 ?
O1 Ba1 O1 180.00(12) 5 2 ?
O1 Ba1 O1 91.21(11) 4 6 ?
O1 Ba1 O1 91.21(11) 5 6 ?
O1 Ba1 O1 88.79(11) 2 6 ?
O1 Ba1 O1 88.79(11) 4 3 ?
O1 Ba1 O1 88.79(11) 5 3 ?
O1 Ba1 O1 91.21(11) 2 3 ?
O1 Ba1 O1 180.00(11) 6 3 ?
O1 Ba1 O1 180.0 4 . ?
O1 Ba1 O1 88.79(11) 5 . ?
O1 Ba1 O1 91.21(11) 2 . ?
O1 Ba1 O1 88.79(11) 6 . ?
O1 Ba1 O1 91.21(11) 3 . ?
C1 O1 Ba1 159.5(3) . . ?
O1 C1 N12 121.1(4) . . ?
O1 C1 N11 120.4(4) . . ?
N12 C1 N11 118.6(4) . . ?
C1 N11 C11 119.2(5) . . ?
C1 N11 C13 122.4(5) . . ?
C11 N11 C13 118.1(5) . . ?
C1 N12 C12 119.2(5) . . ?
C1 N12 C15 122.9(5) . . ?
C12 N12 C15 117.1(5) . . ?
N11 C11 H11A 109.5 . . ?
N11 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N11 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N12 C12 H12A 109.5 . . ?
N12 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N12 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N11 C13 C14 110.4(6) . . ?
N11 C13 H13A 109.6 . . ?
C14 C13 H13A 109.6 . . ?
N11 C13 H13B 109.6 . . ?
C14 C13 H13B 109.6 . . ?
H13A C13 H13B 108.1 . . ?
C15 C14 C13 110.5(6) . . ?
C15 C14 H14A 109.6 . . ?
C13 C14 H14A 109.6 . . ?
C15 C14 H14B 109.6 . . ?
C13 C14 H14B 109.6 . . ?
H14A C14 H14B 108.1 . . ?
C14 C15 N12 110.8(6) . . ?
C14 C15 H15A 109.5 . . ?
N12 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
N12 C15 H15B 109.5 . . ?
H15A C15 H15B 108.1 . . ?
S102 O101 S102 54.7(11) 3_665 . ?
S102 O101 S102 28.0(10) 3_665 2_655 ?
S102 O101 S102 35.3(7) . 2_655 ?
O101 S102 S102 78.1(13) 2_655 2_655 ?
S102 S102 S102 60.0 3_665 2_655 ?
O101 S102 O101 123(3) 2_655 . ?
S102 S102 O101 47.2(8) 3_665 . ?
S102 S102 O101 100.9(10) 2_655 . ?
O101 S102 C103 142(2) 2_655 2_655 ?
S102 S102 C103 61.4(18) 3_665 2_655 ?
S102 S102 C103 78.7(10) 2_655 2_655 ?
O101 S102 C103 90(3) . 2_655 ?
C103 S102 C103 30(4) 3_665 2_655 ?
O101 S102 F104 130(2) 2_655 2_655 ?
S102 S102 F104 100.6(12) 3_665 2_655 ?
S102 S102 F104 122.6(9) 2_655 2_655 ?
O101 S102 F104 98.6(14) . 2_655 ?
C103 S102 F104 50.9(15) 3_665 2_655 ?
C103 S102 F104 47.9(6) 2_655 2_655 ?
O101 S102 C103 119.3(19) 2_655 . ?
S102 S102 C103 60.3(10) 3_665 . ?
S102 S102 C103 54(2) 2_655 . ?
O101 S102 C103 102.5(7) . . ?
C103 S102 C103 25(3) 3_665 . ?
C103 S102 C103 26(3) 2_655 . ?
F104 S102 C103 69(2) 2_655 . ?
C103 C103 F104 75(5) 2_655 . ?
C103 C103 F104 135(5) 3_665 . ?
C103 C103 F104 131(2) 2_655 3_665 ?
C103 C103 F104 71(2) 3_665 3_665 ?
F104 C103 F104 154(5) . 3_665 ?
C103 C103 S102 101.4(14) 2_655 2_655 ?
C103 C103 S102 84.2(16) 3_665 2_655 ?
F104 C103 S102 105(3) . 2_655 ?
F104 C103 S102 72(3) 3_665 2_655 ?
C103 C103 S102 62.4(13) 2_655 . ?
C103 C103 S102 53(2) 3_665 . ?
F104 C103 S102 106.5(8) . . ?
F104 C103 S102 88.3(17) 3_665 . ?
S102 C103 S102 41.7(9) 2_655 . ?
S102 C103 S102 41.0(8) 3_665 . ?
C103 F104 C103 34(4) . 2_655 ?

_refine_diff_density_max         0.958
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.117

####################################################################### 
# 
# 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_Sc_dmpu6_I3
_database_code_depnum_ccdc_archive 'CCDC 2209379'
loop_
_audit_author_name
_audit_author_address
'Lars Eriksson'
;Stockholm University
Sweden
;
_audit_update_record             
;
2023-11-18 deposited with the CCDC.	2023-12-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H72 N12 O6 Sc, 3(I)'
_chemical_formula_sum            'C36 H72 I3 N12 O6 Sc'
_chemical_formula_weight         1194.71

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'
Sc Sc 0.2519 0.3716 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

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

_cell_length_a                   11.9413(10)
_cell_length_b                   12.0708(10)
_cell_length_c                   17.9935(16)
_cell_angle_alpha                90
_cell_angle_beta                 91.590(2)
_cell_angle_gamma                90
_cell_volume                     2592.6(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    5990
_cell_measurement_theta_min      2.02
_cell_measurement_theta_max      28.01

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.35

_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.530
_exptl_crystal_F_000             1200
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_absorpt_coefficient_mu    1.978
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.4699
_exptl_absorpt_correction_T_max  0.5446
_exptl_absorpt_process_details   
; 
Bruker SADABS (1998c) 
;
_exptl_special_details           
;
;
_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART CCD diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17098
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.021
_diffrn_reflns_theta_max         25.681
_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             4932
_reflns_number_gt                3055
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _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 SMART (1998b)'
_computing_cell_refinement       'Bruker SMART and SAINT (1998b)'
_computing_data_reduction        'Bruker SAINT (1998b)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0526P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4932
_refine_ls_number_parameters     271
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0337
_refine_ls_wR_factor_ref         0.0925
_refine_ls_wR_factor_gt          0.0880
_refine_ls_goodness_of_fit_ref   0.902
_refine_ls_restrained_S_all      0.902
_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
I1 I 0.47555(3) 0.02666(3) 0.23532(2) 0.09371(15) Uani 1 1 d . . . . .
I2 I 0.500000 -0.500000 0.500000 0.08633(16) Uani 1 2 d S . P . .
Sc1 Sc 1.000000 0.000000 0.500000 0.03960(19) Uani 1 2 d S . P . .
O21 O 0.91728(16) 0.13359(17) 0.45021(11) 0.0508(5) Uani 1 1 d . . . . .
O1 O 1.05864(18) -0.04501(18) 0.39723(11) 0.0542(6) Uani 1 1 d . . . . .
O11 O 0.86141(16) -0.10114(17) 0.48250(11) 0.0501(5) Uani 1 1 d . . . . .
N22 N 0.7585(2) 0.1992(2) 0.39564(16) 0.0578(7) Uani 1 1 d . . . . .
N21 N 0.8983(2) 0.3189(2) 0.43580(16) 0.0628(8) Uani 1 1 d . . . . .
N12 N 0.6826(2) -0.1382(2) 0.51112(18) 0.0647(8) Uani 1 1 d . . . . .
N2 N 1.1640(2) -0.1560(2) 0.32588(15) 0.0594(7) Uani 1 1 d . . . . .
N11 N 0.7560(2) -0.2022(3) 0.40185(17) 0.0650(8) Uani 1 1 d . . . . .
N1 N 1.0795(3) 0.0011(3) 0.27712(16) 0.0669(8) Uani 1 1 d . . . . .
C24 C 0.6834(3) 0.2885(3) 0.3722(2) 0.0753(11) Uani 1 1 d . . . . .
H24A H 0.631003 0.303665 0.411184 0.090 Uiso 1 1 calc R U . . .
H24B H 0.640748 0.265964 0.328077 0.090 Uiso 1 1 calc R U . . .
C22 C 0.8288(4) 0.4163(3) 0.4182(2) 0.0796(12) Uani 1 1 d . . . . .
H22A H 0.876229 0.477703 0.404266 0.096 Uiso 1 1 calc R U . . .
H22B H 0.788099 0.438152 0.461817 0.096 Uiso 1 1 calc R U . . .
C23 C 0.7480(3) 0.3903(3) 0.3560(2) 0.0832(12) Uani 1 1 d . . . . .
H23A H 0.696784 0.451983 0.348580 0.100 Uiso 1 1 calc R U . . .
H23B H 0.788477 0.379989 0.310502 0.100 Uiso 1 1 calc R U . . .
C21 C 0.8594(3) 0.2162(3) 0.42822(17) 0.0482(8) Uani 1 1 d . . . . .
C1 C 1.0997(3) -0.0660(3) 0.33475(19) 0.0516(8) Uani 1 1 d . . . . .
C11 C 0.7684(3) -0.1463(2) 0.46591(19) 0.0498(8) Uani 1 1 d . . . . .
C4 C 1.2121(4) -0.1871(4) 0.2549(2) 0.0811(12) Uani 1 1 d . . . . .
H4A H 1.211265 -0.267130 0.250056 0.097 Uiso 1 1 calc R U . . .
H4B H 1.289430 -0.162688 0.254163 0.097 Uiso 1 1 calc R U . . .
C6 C 1.1946(4) -0.2255(3) 0.3889(2) 0.0818(12) Uani 1 1 d . . . . .
H6A H 1.167463 -0.299397 0.380163 0.123 Uiso 1 1 calc R U . . .
H6B H 1.162016 -0.196304 0.432928 0.123 Uiso 1 1 calc R U . . .
H6C H 1.274697 -0.227019 0.395274 0.123 Uiso 1 1 calc R U . . .
C26 C 1.0078(4) 0.3400(3) 0.4673(3) 0.0999(15) Uani 1 1 d . . . . .
H26A H 1.047210 0.389838 0.435766 0.150 Uiso 1 1 calc R U . . .
H26B H 1.048427 0.271530 0.471719 0.150 Uiso 1 1 calc R U . . .
H26C H 1.001113 0.372589 0.515673 0.150 Uiso 1 1 calc R U . . .
C2 C 1.1309(4) -0.0170(4) 0.2052(2) 0.0932(14) Uani 1 1 d . . . . .
H2A H 1.202217 0.021481 0.204409 0.112 Uiso 1 1 calc R U . . .
H2B H 1.082847 0.013490 0.166001 0.112 Uiso 1 1 calc R U . . .
C12 C 0.5726(3) -0.1846(4) 0.4939(3) 0.0932(14) Uani 1 1 d . . . . .
H12A H 0.515357 -0.135962 0.512866 0.112 Uiso 1 1 calc R U . . .
H12B H 0.565726 -0.255921 0.518210 0.112 Uiso 1 1 calc R U . . .
C25 C 0.7126(3) 0.0891(3) 0.3910(3) 0.0924(14) Uani 1 1 d . . . . .
H25A H 0.649579 0.088539 0.356769 0.139 Uiso 1 1 calc R U . . .
H25B H 0.688964 0.066316 0.439261 0.139 Uiso 1 1 calc R U . . .
H25C H 0.768782 0.038873 0.374038 0.139 Uiso 1 1 calc R U . . .
C14 C 0.6497(4) -0.2553(4) 0.3801(3) 0.1005(16) Uani 1 1 d . . . . .
H14A H 0.641113 -0.254747 0.326329 0.121 Uiso 1 1 calc R U . . .
H14B H 0.650887 -0.331837 0.396432 0.121 Uiso 1 1 calc R U . . .
C13 C 0.5547(4) -0.1986(4) 0.4123(3) 0.1099(18) Uani 1 1 d . . . . .
H13A H 0.486996 -0.241156 0.402591 0.132 Uiso 1 1 calc R U . . .
H13B H 0.545158 -0.126496 0.389170 0.132 Uiso 1 1 calc R U . . .
C16 C 0.8489(4) -0.2160(4) 0.3525(2) 0.0915(14) Uani 1 1 d . . . . .
H16A H 0.844103 -0.287467 0.329196 0.137 Uiso 1 1 calc R U . . .
H16B H 0.918246 -0.210316 0.380489 0.137 Uiso 1 1 calc R U . . .
H16C H 0.845834 -0.159345 0.315016 0.137 Uiso 1 1 calc R U . . .
C3 C 1.1490(4) -0.1374(4) 0.1913(2) 0.0999(15) Uani 1 1 d . . . . .
H3A H 1.077277 -0.174337 0.184710 0.120 Uiso 1 1 calc R U . . .
H3B H 1.190530 -0.147048 0.146208 0.120 Uiso 1 1 calc R U . . .
C15 C 0.6974(4) -0.0866(4) 0.5829(2) 0.0953(14) Uani 1 1 d . . . . .
H15A H 0.636337 -0.106738 0.613810 0.143 Uiso 1 1 calc R U . . .
H15B H 0.699058 -0.007592 0.577076 0.143 Uiso 1 1 calc R U . . .
H15C H 0.766645 -0.111160 0.605764 0.143 Uiso 1 1 calc R U . . .
C5 C 1.0161(4) 0.1012(4) 0.2863(2) 0.1003(16) Uani 1 1 d . . . . .
H5A H 1.054727 0.161935 0.263957 0.151 Uiso 1 1 calc R U . . .
H5B H 1.007733 0.115633 0.338284 0.151 Uiso 1 1 calc R U . . .
H5C H 0.943499 0.092888 0.262657 0.151 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sc1 O1 2.068(2) . ?
Sc1 O1 2.068(2) 3_756 ?
Sc1 O11 2.073(2) 3_756 ?
Sc1 O11 2.0735(19) . ?
Sc1 O21 2.0807(19) 3_756 ?
Sc1 O21 2.0808(19) . ?
O21 C21 1.270(3) . ?
O1 C1 1.265(4) . ?
O11 C11 1.265(3) . ?
N22 C21 1.341(4) . ?
N22 C25 1.439(5) . ?
N22 C24 1.457(4) . ?
N21 C21 1.330(4) . ?
N21 C26 1.434(4) . ?
N21 C22 1.469(4) . ?
N12 C11 1.330(4) . ?
N12 C15 1.441(5) . ?
N12 C12 1.453(5) . ?
N2 C1 1.342(4) . ?
N2 C6 1.449(4) . ?
N2 C4 1.464(4) . ?
N11 C11 1.340(4) . ?
N11 C16 1.450(5) . ?
N11 C14 1.465(5) . ?
N1 C1 1.332(4) . ?
N1 C5 1.438(5) . ?
N1 C2 1.463(5) . ?
C24 C23 1.485(5) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C22 C23 1.492(5) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C4 C3 1.479(6) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C2 C3 1.492(6) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C12 C13 1.487(6) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C14 C13 1.459(6) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Sc1 O1 180.00(12) . 3_756 ?
O1 Sc1 O11 90.11(8) . 3_756 ?
O1 Sc1 O11 89.89(8) 3_756 3_756 ?
O1 Sc1 O11 89.89(8) . . ?
O1 Sc1 O11 90.11(8) 3_756 . ?
O11 Sc1 O11 180.0 3_756 . ?
O1 Sc1 O21 90.74(8) . 3_756 ?
O1 Sc1 O21 89.26(8) 3_756 3_756 ?
O11 Sc1 O21 91.35(8) 3_756 3_756 ?
O11 Sc1 O21 88.65(8) . 3_756 ?
O1 Sc1 O21 89.26(8) . . ?
O1 Sc1 O21 90.74(8) 3_756 . ?
O11 Sc1 O21 88.65(8) 3_756 . ?
O11 Sc1 O21 91.35(8) . . ?
O21 Sc1 O21 180.0 3_756 . ?
C21 O21 Sc1 172.0(2) . . ?
C1 O1 Sc1 175.4(2) . . ?
C11 O11 Sc1 168.9(2) . . ?
C21 N22 C25 120.1(3) . . ?
C21 N22 C24 123.5(3) . . ?
C25 N22 C24 115.9(3) . . ?
C21 N21 C26 121.2(3) . . ?
C21 N21 C22 122.1(3) . . ?
C26 N21 C22 116.6(3) . . ?
C11 N12 C15 120.2(3) . . ?
C11 N12 C12 123.3(3) . . ?
C15 N12 C12 116.5(3) . . ?
C1 N2 C6 120.6(3) . . ?
C1 N2 C4 123.4(3) . . ?
C6 N2 C4 115.9(3) . . ?
C11 N11 C16 121.1(3) . . ?
C11 N11 C14 121.6(3) . . ?
C16 N11 C14 117.2(3) . . ?
C1 N1 C5 120.4(3) . . ?
C1 N1 C2 121.7(3) . . ?
C5 N1 C2 117.5(3) . . ?
N22 C24 C23 110.5(3) . . ?
N22 C24 H24A 109.5 . . ?
C23 C24 H24A 109.5 . . ?
N22 C24 H24B 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 108.1 . . ?
N21 C22 C23 110.1(3) . . ?
N21 C22 H22A 109.7 . . ?
C23 C22 H22A 109.7 . . ?
N21 C22 H22B 109.7 . . ?
C23 C22 H22B 109.7 . . ?
H22A C22 H22B 108.2 . . ?
C24 C23 C22 110.8(3) . . ?
C24 C23 H23A 109.5 . . ?
C22 C23 H23A 109.5 . . ?
C24 C23 H23B 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 108.1 . . ?
O21 C21 N21 121.0(3) . . ?
O21 C21 N22 119.4(3) . . ?
N21 C21 N22 119.6(3) . . ?
O1 C1 N1 120.2(3) . . ?
O1 C1 N2 120.3(3) . . ?
N1 C1 N2 119.4(3) . . ?
O11 C11 N12 120.7(3) . . ?
O11 C11 N11 119.7(3) . . ?
N12 C11 N11 119.6(3) . . ?
N2 C4 C3 111.5(4) . . ?
N2 C4 H4A 109.3 . . ?
C3 C4 H4A 109.3 . . ?
N2 C4 H4B 109.3 . . ?
C3 C4 H4B 109.3 . . ?
H4A C4 H4B 108.0 . . ?
N2 C6 H6A 109.5 . . ?
N2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N21 C26 H26A 109.5 . . ?
N21 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
N21 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N1 C2 C3 111.1(4) . . ?
N1 C2 H2A 109.4 . . ?
C3 C2 H2A 109.4 . . ?
N1 C2 H2B 109.4 . . ?
C3 C2 H2B 109.4 . . ?
H2A C2 H2B 108.0 . . ?
N12 C12 C13 111.0(3) . . ?
N12 C12 H12A 109.4 . . ?
C13 C12 H12A 109.4 . . ?
N12 C12 H12B 109.4 . . ?
C13 C12 H12B 109.4 . . ?
H12A C12 H12B 108.0 . . ?
N22 C25 H25A 109.5 . . ?
N22 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
N22 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C13 C14 N11 111.5(4) . . ?
C13 C14 H14A 109.3 . . ?
N11 C14 H14A 109.3 . . ?
C13 C14 H14B 109.3 . . ?
N11 C14 H14B 109.3 . . ?
H14A C14 H14B 108.0 . . ?
C14 C13 C12 110.7(4) . . ?
C14 C13 H13A 109.5 . . ?
C12 C13 H13A 109.5 . . ?
C14 C13 H13B 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 108.1 . . ?
N11 C16 H16A 109.5 . . ?
N11 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
N11 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C4 C3 C2 109.8(4) . . ?
C4 C3 H3A 109.7 . . ?
C2 C3 H3A 109.7 . . ?
C4 C3 H3B 109.7 . . ?
C2 C3 H3B 109.7 . . ?
H3A C3 H3B 108.2 . . ?
N12 C15 H15A 109.5 . . ?
N12 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
N12 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N1 C5 H5A 109.5 . . ?
N1 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N1 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C21 N22 C24 C23 26.4(5) . . . . ?
C25 N22 C24 C23 -161.6(4) . . . . ?
C21 N21 C22 C23 -32.4(5) . . . . ?
C26 N21 C22 C23 152.5(4) . . . . ?
N22 C24 C23 C22 -49.7(5) . . . . ?
N21 C22 C23 C24 52.6(5) . . . . ?
C26 N21 C21 O21 1.5(5) . . . . ?
C22 N21 C21 O21 -173.3(3) . . . . ?
C26 N21 C21 N22 -177.2(4) . . . . ?
C22 N21 C21 N22 7.9(5) . . . . ?
C25 N22 C21 O21 4.9(5) . . . . ?
C24 N22 C21 O21 176.6(3) . . . . ?
C25 N22 C21 N21 -176.3(3) . . . . ?
C24 N22 C21 N21 -4.6(5) . . . . ?
C5 N1 C1 O1 3.5(5) . . . . ?
C2 N1 C1 O1 176.3(3) . . . . ?
C5 N1 C1 N2 -176.5(4) . . . . ?
C2 N1 C1 N2 -3.7(5) . . . . ?
C6 N2 C1 O1 -4.9(5) . . . . ?
C4 N2 C1 O1 178.4(3) . . . . ?
C6 N2 C1 N1 175.1(3) . . . . ?
C4 N2 C1 N1 -1.6(5) . . . . ?
Sc1 O11 C11 N12 -86.1(12) . . . . ?
Sc1 O11 C11 N11 93.3(11) . . . . ?
C15 N12 C11 O11 -5.9(5) . . . . ?
C12 N12 C11 O11 177.6(3) . . . . ?
C15 N12 C11 N11 174.7(3) . . . . ?
C12 N12 C11 N11 -1.8(5) . . . . ?
C16 N11 C11 O11 2.8(5) . . . . ?
C14 N11 C11 O11 -179.6(4) . . . . ?
C16 N11 C11 N12 -177.8(3) . . . . ?
C14 N11 C11 N12 -0.2(5) . . . . ?
C1 N2 C4 C3 -22.1(5) . . . . ?
C6 N2 C4 C3 161.1(4) . . . . ?
C1 N1 C2 C3 31.8(6) . . . . ?
C5 N1 C2 C3 -155.2(4) . . . . ?
C11 N12 C12 C13 -23.3(6) . . . . ?
C15 N12 C12 C13 160.0(4) . . . . ?
C11 N11 C14 C13 27.8(6) . . . . ?
C16 N11 C14 C13 -154.5(4) . . . . ?
N11 C14 C13 C12 -51.5(5) . . . . ?
N12 C12 C13 C14 49.3(5) . . . . ?
N2 C4 C3 C2 48.3(5) . . . . ?
N1 C2 C3 C4 -53.1(5) . . . . ?

_refine_diff_density_max         0.988
_refine_diff_density_min         -0.580
_refine_diff_density_rms         0.060

####################################################################### 
# 
# 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_r_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 2249334'
loop_
_audit_author_name
_audit_author_address
'Lars Eriksson'
;Stockholm University
Sweden
;
_audit_update_record             
;
2023-11-18 deposited with the CCDC.	2023-12-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C19 H36 F3 N6 O6 S Sr0.50'
_chemical_formula_weight         577.41

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sr Sr -1.5307 3.2498 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_H-M_alt        'P -3'
_space_group_name_Hall           '-P 3'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'

_cell_length_a                   13.7677(7)
_cell_length_b                   13.7677(7)
_cell_length_c                   8.5413(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1402.09(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    999
_cell_measurement_theta_min      3.45
_cell_measurement_theta_max      25.00

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_F_000             604
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    1.118
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.83
_exptl_absorpt_correction_T_max  0.89
_exptl_absorpt_process_details   'Bruker SADABS (1998)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker SMART CCD diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            4522
_diffrn_reflns_av_unetI/netI     0.0577
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         3.417
_diffrn_reflns_theta_max         25.645
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measured_fraction_theta_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_point_group_measured_fraction_full 0.978
_reflns_number_total             1734
_reflns_number_gt                1464
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _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 SMART (1998b)'
_computing_cell_refinement       '(Bruker SMART and SAINT (1998b)'
_computing_data_reduction        '(Bruker SAINT (1998b)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.1770P)²+4.3389P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1734
_refine_ls_number_parameters     110
_refine_ls_number_restraints     89
_refine_ls_R_factor_all          0.1150
_refine_ls_R_factor_gt           0.1017
_refine_ls_wR_factor_ref         0.2769
_refine_ls_wR_factor_gt          0.2620
_refine_ls_goodness_of_fit_ref   0.928
_refine_ls_restrained_S_all      0.913
_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
Sr1 Sr 0.000000 0.000000 0.000000 0.0440(5) Uani 1 6 d S TU P . .
O1 O -0.0687(4) -0.1695(4) -0.1642(6) 0.0704(14) Uani 1 1 d . U . . .
C1 C -0.0831(6) -0.2590(6) -0.2172(8) 0.0579(16) Uani 1 1 d . U . . .
N11 N -0.1781(6) -0.3562(5) -0.1852(8) 0.0772(19) Uani 1 1 d . U . . .
N12 N -0.0065(6) -0.2631(6) -0.3103(8) 0.0725(17) Uani 1 1 d . U . . .
C11 C -0.2662(9) -0.3527(9) -0.0976(15) 0.120(4) Uani 1 1 d . U . . .
H11A H -0.241166 -0.276996 -0.065338 0.180 Uiso 1 1 calc R U . . .
H11B H -0.284274 -0.399821 -0.006865 0.180 Uiso 1 1 calc R U . . .
H11C H -0.331528 -0.378904 -0.162367 0.180 Uiso 1 1 calc R U . . .
C12 C 0.0897(9) -0.1604(9) -0.3594(15) 0.113(4) Uani 1 1 d . U . . .
H12A H 0.066271 -0.109006 -0.394461 0.169 Uiso 1 1 calc R U . . .
H12B H 0.126549 -0.175374 -0.443535 0.169 Uiso 1 1 calc R U . . .
H12C H 0.140590 -0.127968 -0.273050 0.169 Uiso 1 1 calc R U . . .
C13 C -0.0218(9) -0.3669(8) -0.3770(13) 0.093(3) Uani 1 1 d . U . . .
H13A H 0.050449 -0.362622 -0.385489 0.111 Uiso 1 1 calc R U . . .
H13B H -0.052688 -0.376150 -0.481653 0.111 Uiso 1 1 calc R U . . .
C14 C -0.0966(13) -0.4638(9) -0.2821(16) 0.120(4) Uani 1 1 d . U . . .
H14A H -0.113534 -0.532085 -0.337369 0.144 Uiso 1 1 calc R U . . .
H14B H -0.059648 -0.462148 -0.184588 0.144 Uiso 1 1 calc R U . . .
C15 C -0.1997(11) -0.4638(7) -0.2489(14) 0.111(4) Uani 1 1 d . U . . .
H15A H -0.243779 -0.522862 -0.174443 0.133 Uiso 1 1 calc R U . . .
H15B H -0.243116 -0.479482 -0.344520 0.133 Uiso 1 1 calc R U . . .
S10 S -0.333333 -0.666667 -0.6550(17) 0.342(10) Uani 1 3 d DS TU P . .
O10 O -0.248(3) -0.5541(11) -0.6158(17) 0.75(5) Uani 1 1 d D U . . .
C10 C -0.333333 -0.666667 -0.8680(17) 0.54(7) Uani 1 3 d DS TU P . .
F10 F -0.382(4) -0.7703(2) -0.9253(17) 0.65(4) Uani 1 1 d D U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sr1 O1 2.470(5) . ?
Sr1 O1 2.470(5) 4 ?
Sr1 O1 2.470(5) 6 ?
Sr1 O1 2.470(5) 3 ?
Sr1 O1 2.470(5) 2 ?
Sr1 O1 2.470(5) 5 ?
O1 C1 1.232(8) . ?
C1 N12 1.345(9) . ?
C1 N11 1.351(9) . ?
N11 C11 1.447(12) . ?
N11 C15 1.462(11) . ?
N12 C12 1.435(12) . ?
N12 C13 1.452(11) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 C14 1.458(16) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 C15 1.448(17) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
S10 O10 1.4400(11) 2_445 ?
S10 O10 1.4401(10) . ?
S10 O10 1.4401(10) 3_545 ?
S10 C10 1.8201(10) . ?
C10 F10 1.3301(11) 2_445 ?
C10 F10 1.3301(11) . ?
C10 F10 1.3302(10) 3_545 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Sr1 O1 180.0 . 4 ?
O1 Sr1 O1 89.06(18) . 6 ?
O1 Sr1 O1 90.94(18) 4 6 ?
O1 Sr1 O1 90.94(18) . 3 ?
O1 Sr1 O1 89.06(18) 4 3 ?
O1 Sr1 O1 180.0(3) 6 3 ?
O1 Sr1 O1 90.94(18) . 2 ?
O1 Sr1 O1 89.06(18) 4 2 ?
O1 Sr1 O1 89.06(18) 6 2 ?
O1 Sr1 O1 90.94(18) 3 2 ?
O1 Sr1 O1 89.06(18) . 5 ?
O1 Sr1 O1 90.94(18) 4 5 ?
O1 Sr1 O1 90.94(18) 6 5 ?
O1 Sr1 O1 89.06(18) 3 5 ?
O1 Sr1 O1 180.0(4) 2 5 ?
C1 O1 Sr1 161.4(5) . . ?
O1 C1 N12 121.5(7) . . ?
O1 C1 N11 120.6(7) . . ?
N12 C1 N11 117.9(6) . . ?
C1 N11 C11 118.9(7) . . ?
C1 N11 C15 122.3(7) . . ?
C11 N11 C15 118.5(8) . . ?
C1 N12 C12 119.2(7) . . ?
C1 N12 C13 122.9(7) . . ?
C12 N12 C13 117.6(7) . . ?
N11 C11 H11A 109.5 . . ?
N11 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N11 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N12 C12 H12A 109.5 . . ?
N12 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N12 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N12 C13 C14 111.8(8) . . ?
N12 C13 H13A 109.3 . . ?
C14 C13 H13A 109.3 . . ?
N12 C13 H13B 109.3 . . ?
C14 C13 H13B 109.3 . . ?
H13A C13 H13B 107.9 . . ?
C15 C14 C13 110.6(9) . . ?
C15 C14 H14A 109.5 . . ?
C13 C14 H14A 109.5 . . ?
C15 C14 H14B 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 108.1 . . ?
C14 C15 N11 111.7(9) . . ?
C14 C15 H15A 109.3 . . ?
N11 C15 H15A 109.3 . . ?
C14 C15 H15B 109.3 . . ?
N11 C15 H15B 109.3 . . ?
H15A C15 H15B 107.9 . . ?
O10 S10 O10 114.78(7) 2_445 . ?
O10 S10 O10 114.78(7) 2_445 3_545 ?
O10 S10 O10 114.78(7) . 3_545 ?
O10 S10 C10 103.43(9) 2_445 . ?
O10 S10 C10 103.43(9) . . ?
O10 S10 C10 103.43(9) 3_545 . ?
F10 C10 F10 107.28(11) 2_445 . ?
F10 C10 F10 107.28(12) 2_445 3_545 ?
F10 C10 F10 107.28(12) . 3_545 ?
F10 C10 S10 111.59(11) 2_445 . ?
F10 C10 S10 111.58(11) . . ?
F10 C10 S10 111.58(11) 3_545 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Sr1 O1 C1 N12 -78.0(17) . . . . ?
Sr1 O1 C1 N11 103.1(16) . . . . ?
O1 C1 N11 C11 4.7(12) . . . . ?
N12 C1 N11 C11 -174.3(9) . . . . ?
O1 C1 N11 C15 178.4(9) . . . . ?
N12 C1 N11 C15 -0.5(12) . . . . ?
O1 C1 N12 C12 -5.2(12) . . . . ?
N11 C1 N12 C12 173.7(8) . . . . ?
O1 C1 N12 C13 -178.9(7) . . . . ?
N11 C1 N12 C13 0.1(11) . . . . ?
C1 N12 C13 C14 -26.0(13) . . . . ?
C12 N12 C13 C14 160.3(10) . . . . ?
N12 C13 C14 C15 51.0(13) . . . . ?
C13 C14 C15 N11 -51.3(14) . . . . ?
C1 N11 C15 C14 27.0(15) . . . . ?
C11 N11 C15 C14 -159.2(11) . . . . ?
O10 S10 C10 F10 161(3) 2_445 . . 2_445 ?
O10 S10 C10 F10 41(3) . . . 2_445 ?
O10 S10 C10 F10 -79(3) 3_545 . . 2_445 ?
O10 S10 C10 F10 -79(3) 2_445 . . . ?
O10 S10 C10 F10 161(3) . . . . ?
O10 S10 C10 F10 41(3) 3_545 . . . ?
O10 S10 C10 F10 41(3) 2_445 . . 3_545 ?
O10 S10 C10 F10 -79(3) . . . 3_545 ?
O10 S10 C10 F10 161(3) 3_545 . . 3_545 ?

_refine_diff_density_max         1.454
_refine_diff_density_min         -0.991
_refine_diff_density_rms         0.117

####################################################################### 
# 
# 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_Co_dmpu2_Br2
_database_code_depnum_ccdc_archive 'CCDC 2209424'
loop_
_audit_author_name
_audit_author_address
'Lars Eriksson'
;Stockholm University
Sweden
;
_audit_update_record             
;
2022-09-26 deposited with the CCDC.	2023-12-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H24 Br2 Co N4 O2'
_chemical_formula_sum            'C12 H24 Br2 Co N4 O2'
_chemical_formula_weight         475.10

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 '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'

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

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

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

_cell_length_a                   8.0226(15)
_cell_length_b                   8.4660(16)
_cell_length_c                   26.796(5)
_cell_angle_alpha                90
_cell_angle_beta                 92.364(2)
_cell_angle_gamma                90
_cell_volume                     1818.4(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    3012
_cell_measurement_theta_max      24.09
_cell_measurement_theta_min      2.52

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.735
_exptl_crystal_F_000             948
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_exptl_absorpt_coefficient_mu    5.347
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.5789
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker (2004)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_source                   'sealed tube'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8656
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.523
_diffrn_reflns_theta_max         24.812
_diffrn_reflns_theta_full        24.812
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             3117
_reflns_number_gt                2471
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _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_cell_refinement       'CrysAlis PRO'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'CrysAlis PRO'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0309P)²+0.7471P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.0021(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3117
_refine_ls_number_parameters     205
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0311
_refine_ls_wR_factor_ref         0.0739
_refine_ls_wR_factor_gt          0.0696
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.81443(6) 0.80037(5) 0.37911(2) 0.04101(15) Uani 1 1 d . . . . .
Br1 Br 1.05975(5) 0.94172(5) 0.35945(2) 0.06488(16) Uani 1 1 d . . . . .
Br2 Br 0.83809(6) 0.52299(5) 0.39128(2) 0.07045(17) Uani 1 1 d . . . . .
O1 O 0.6547(3) 0.8555(3) 0.32409(8) 0.0521(6) Uani 1 1 d . . . . .
C1 C 0.6932(4) 0.9178(4) 0.28314(12) 0.0434(8) Uani 1 1 d . . . . .
N11 N 0.6823(4) 1.0736(4) 0.27681(11) 0.0542(8) Uani 1 1 d . . . . .
N12 N 0.7394(4) 0.8266(3) 0.24560(10) 0.0484(7) Uani 1 1 d . . . . .
C11 C 0.6508(7) 1.1728(5) 0.31970(18) 0.0921(17) Uani 1 1 d . . . . .
H11A H 0.598024 1.268993 0.308564 0.138 Uiso 1 1 calc R U . . .
H11B H 0.754538 1.196913 0.337181 0.138 Uiso 1 1 calc R U . . .
H11C H 0.579074 1.117881 0.341665 0.138 Uiso 1 1 calc R U . . .
C12 C 0.7573(5) 0.6571(5) 0.25292(16) 0.0669(12) Uani 1 1 d . . . . .
H12A H 0.748091 0.604666 0.221171 0.100 Uiso 1 1 calc R U . . .
H12B H 0.671169 0.619864 0.273794 0.100 Uiso 1 1 calc R U . . .
H12C H 0.864450 0.635025 0.268642 0.100 Uiso 1 1 calc R U . . .
C13 C 0.7271(6) 1.1530(5) 0.23130(17) 0.0716(12) Uani 1 1 d . . . . .
H13A H 0.840267 1.192876 0.235270 0.086 Uiso 1 1 calc R U . . .
H13B H 0.653329 1.242321 0.225194 0.086 Uiso 1 1 calc R U . . .
C14 C 0.8007(6) 0.8919(5) 0.19998(14) 0.0700(12) Uani 1 1 d . . . . .
H14A H 0.781357 0.817353 0.172864 0.084 Uiso 1 1 calc R U . . .
H14B H 0.919931 0.909817 0.203965 0.084 Uiso 1 1 calc R U . . .
C15 C 0.7150(6) 1.0433(5) 0.18755(15) 0.0742(13) Uani 1 1 d . . . . .
H15A H 0.598610 1.023056 0.178527 0.089 Uiso 1 1 calc R U . . .
H15B H 0.765901 1.091834 0.159143 0.089 Uiso 1 1 calc R U . . .
O2 O 0.7214(3) 0.8809(3) 0.44035(8) 0.0548(7) Uani 1 1 d . . . . .
C2 C 0.6761(5) 0.8100(4) 0.47910(13) 0.0439(9) Uani 1 1 d . . . . .
N21 N 0.7891(4) 0.7640(4) 0.51431(10) 0.0521(8) Uani 1 1 d . . . . .
N22 N 0.5147(4) 0.7864(4) 0.48574(10) 0.0502(8) Uani 1 1 d . . . . .
C21 C 0.9662(5) 0.7821(6) 0.50730(17) 0.0758(13) Uani 1 1 d . . . . .
H21A H 1.018598 0.826958 0.536860 0.114 Uiso 1 1 calc R U . . .
H21B H 0.982776 0.850568 0.479390 0.114 Uiso 1 1 calc R U . . .
H21C H 1.014445 0.680612 0.500986 0.114 Uiso 1 1 calc R U . . .
C22 C 0.3913(5) 0.8252(5) 0.44656(16) 0.0688(12) Uani 1 1 d . . . . .
H22A H 0.319659 0.735959 0.440315 0.103 Uiso 1 1 calc R U . . .
H22B H 0.446591 0.851912 0.416607 0.103 Uiso 1 1 calc R U . . .
H22C H 0.325934 0.913567 0.456837 0.103 Uiso 1 1 calc R U . . .
C23 C 0.7405(6) 0.6793(6) 0.55830(17) 0.0826(15) Uani 1 1 d . . . . .
H23A H 0.739827 0.566858 0.551357 0.099 Uiso 0.58(2) 1 calc R U P A 1
H23B H 0.821885 0.698711 0.585375 0.099 Uiso 0.58(2) 1 calc R U P A 1
H23C H 0.769269 0.744392 0.587175 0.099 Uiso 0.42(2) 1 calc R U P A 2
H23D H 0.808003 0.584444 0.561113 0.099 Uiso 0.42(2) 1 calc R U P A 2
C24A C 0.5814(12) 0.726(2) 0.5733(3) 0.060(3) Uani 0.58(2) 1 d . . P A 1
H24A H 0.589271 0.830952 0.587371 0.072 Uiso 0.58(2) 1 calc R U P A 1
H24B H 0.547169 0.654784 0.599439 0.072 Uiso 0.58(2) 1 calc R U P A 1
C24B C 0.5668(16) 0.633(3) 0.5614(7) 0.068(5) Uani 0.42(2) 1 d . . P A 2
H24C H 0.556044 0.523309 0.551157 0.081 Uiso 0.42(2) 1 calc R U P A 2
H24D H 0.536862 0.638957 0.596087 0.081 Uiso 0.42(2) 1 calc R U P A 2
C25 C 0.4496(5) 0.7253(5) 0.53190(15) 0.0627(11) Uani 1 1 d . . . . .
H25A H 0.409423 0.618368 0.526456 0.075 Uiso 0.58(2) 1 calc R U P A 1
H25B H 0.356233 0.789767 0.541473 0.075 Uiso 0.58(2) 1 calc R U P A 1
H25C H 0.413448 0.813537 0.551851 0.075 Uiso 0.42(2) 1 calc R U P A 2
H25D H 0.352388 0.660801 0.523690 0.075 Uiso 0.42(2) 1 calc R U 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
Co1 O2 1.953(2) . ?
Co1 O1 1.969(2) . ?
Co1 Br2 2.3773(7) . ?
Co1 Br1 2.3809(7) . ?
O1 C1 1.267(4) . ?
C1 N11 1.332(5) . ?
C1 N12 1.333(4) . ?
N11 C13 1.451(5) . ?
N11 C11 1.454(5) . ?
N12 C14 1.446(5) . ?
N12 C12 1.454(5) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 C15 1.496(6) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 C15 1.486(6) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
O2 C2 1.266(4) . ?
C2 N22 1.330(4) . ?
C2 N21 1.339(4) . ?
N21 C23 1.447(5) . ?
N21 C21 1.449(5) . ?
N22 C22 1.451(5) . ?
N22 C25 1.457(4) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 C24A 1.409(10) . ?
C23 C24B 1.454(15) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C23 H23C 0.9700 . ?
C23 H23D 0.9700 . ?
C24A C25 1.500(11) . ?
C24A H24A 0.9700 . ?
C24A H24B 0.9700 . ?
C24B C25 1.436(14) . ?
C24B H24C 0.9700 . ?
C24B H24D 0.9700 . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C25 H25C 0.9700 . ?
C25 H25D 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Co1 O1 106.67(10) . . ?
O2 Co1 Br2 105.12(7) . . ?
O1 Co1 Br2 112.51(8) . . ?
O2 Co1 Br1 110.99(8) . . ?
O1 Co1 Br1 103.49(7) . . ?
Br2 Co1 Br1 117.70(3) . . ?
C1 O1 Co1 124.9(2) . . ?
O1 C1 N11 120.3(3) . . ?
O1 C1 N12 119.9(3) . . ?
N11 C1 N12 119.8(3) . . ?
C1 N11 C13 123.3(3) . . ?
C1 N11 C11 118.9(3) . . ?
C13 N11 C11 117.0(4) . . ?
C1 N12 C14 122.1(3) . . ?
C1 N12 C12 119.9(3) . . ?
C14 N12 C12 117.1(3) . . ?
N11 C11 H11A 109.5 . . ?
N11 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N11 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N12 C12 H12A 109.5 . . ?
N12 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N12 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N11 C13 C15 111.1(3) . . ?
N11 C13 H13A 109.4 . . ?
C15 C13 H13A 109.4 . . ?
N11 C13 H13B 109.4 . . ?
C15 C13 H13B 109.4 . . ?
H13A C13 H13B 108.0 . . ?
N12 C14 C15 110.4(3) . . ?
N12 C14 H14A 109.6 . . ?
C15 C14 H14A 109.6 . . ?
N12 C14 H14B 109.6 . . ?
C15 C14 H14B 109.6 . . ?
H14A C14 H14B 108.1 . . ?
C14 C15 C13 110.2(4) . . ?
C14 C15 H15A 109.6 . . ?
C13 C15 H15A 109.6 . . ?
C14 C15 H15B 109.6 . . ?
C13 C15 H15B 109.6 . . ?
H15A C15 H15B 108.1 . . ?
C2 O2 Co1 131.0(2) . . ?
O2 C2 N22 119.7(3) . . ?
O2 C2 N21 120.4(3) . . ?
N22 C2 N21 119.8(3) . . ?
C2 N21 C23 121.4(3) . . ?
C2 N21 C21 121.1(3) . . ?
C23 N21 C21 117.2(3) . . ?
C2 N22 C22 120.5(3) . . ?
C2 N22 C25 123.5(3) . . ?
C22 N22 C25 115.9(3) . . ?
N21 C21 H21A 109.5 . . ?
N21 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
N21 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N22 C22 H22A 109.5 . . ?
N22 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
N22 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24A C23 N21 111.9(5) . . ?
N21 C23 C24B 118.2(6) . . ?
C24A C23 H23A 109.2 . . ?
N21 C23 H23A 109.2 . . ?
C24A C23 H23B 109.2 . . ?
N21 C23 H23B 109.2 . . ?
H23A C23 H23B 107.9 . . ?
N21 C23 H23C 107.8 . . ?
C24B C23 H23C 107.8 . . ?
N21 C23 H23D 107.8 . . ?
C24B C23 H23D 107.8 . . ?
H23C C23 H23D 107.1 . . ?
C23 C24A C25 114.1(7) . . ?
C23 C24A H24A 108.7 . . ?
C25 C24A H24A 108.7 . . ?
C23 C24A H24B 108.7 . . ?
C25 C24A H24B 108.7 . . ?
H24A C24A H24B 107.6 . . ?
C25 C24B C23 115.3(10) . . ?
C25 C24B H24C 108.4 . . ?
C23 C24B H24C 108.4 . . ?
C25 C24B H24D 108.4 . . ?
C23 C24B H24D 108.4 . . ?
H24C C24B H24D 107.5 . . ?
C24B C25 N22 114.4(6) . . ?
N22 C25 C24A 111.2(5) . . ?
N22 C25 H25A 109.4 . . ?
C24A C25 H25A 109.4 . . ?
N22 C25 H25B 109.4 . . ?
C24A C25 H25B 109.4 . . ?
H25A C25 H25B 108.0 . . ?
C24B C25 H25C 108.7 . . ?
N22 C25 H25C 108.7 . . ?
C24B C25 H25D 108.7 . . ?
N22 C25 H25D 108.7 . . ?
H25C C25 H25D 107.6 . . ?

_refine_diff_density_max         0.461
_refine_diff_density_min         -0.531
_refine_diff_density_rms         0.061

