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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mgspp
_database_code_depnum_ccdc_archive 'CCDC 1968802'
loop_
_audit_author_name
_audit_author_address
'Stephan Woehlbrandt'
;Institut fuer Anorganische Chemie, Universitaet Kiel
Germany
;
_audit_update_record             
;
2020-02-04 deposited with the CCDC.	2020-02-07 downloaded from the CCDC.
;
_audit_creation_date             2019-08-08
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C9 H17 Mg N O11 P2 S, H2 O'
_chemical_formula_sum            'C9 H19 Mg N O12 P2 S'
_chemical_formula_weight         451.56
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mg Mg 0.0486 0.0363 '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'
P P 0.1023 0.0942 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   7.6543(15)
_cell_length_b                   8.0979(16)
_cell_length_c                   26.554(5)
_cell_angle_alpha                90
_cell_angle_beta                 90.64(3)
_cell_angle_gamma                90
_cell_volume                     1645.8(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    25064
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      3.1
_cell_measurement_theta_min      54.9
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.496
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.9984
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-RED and X-SHAPE (STOE, 2008)'
_exptl_crystal_colour            white
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.822
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0425
_diffrn_reflns_av_unetI/netI     0.0199
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            24123
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.433
_diffrn_reflns_theta_min         1.534
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'STOE IPDS-2'
_diffrn_measurement_method       'Omega scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3489
_reflns_number_total             3752
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'X-Area (STOE 2007)'
_computing_data_collection       'X-Area (STOE 2007)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2014)'
_refine_diff_density_max         0.397
_refine_diff_density_min         -0.520
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         3752
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0322
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0506P)²+1.1650P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0861
_refine_ls_wR_factor_ref         0.0880
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
Mg1 Mg -0.20452(7) 0.29273(7) 0.29669(2) 0.01592(13) Uani 1 1 d . . . . .
O1 O -0.07223(19) 0.10622(18) 0.33662(6) 0.0286(3) Uani 1 1 d . . . . .
H1A H -0.016(4) 0.125(4) 0.3654(12) 0.047(8) Uiso 1 1 d . . . . .
H1B H -0.065(4) 0.017(4) 0.3287(13) 0.058(10) Uiso 1 1 d . . . . .
O2 O -0.33164(19) 0.35579(18) 0.36226(5) 0.0261(3) Uani 1 1 d . . . . .
H2A H -0.276(4) 0.405(4) 0.3858(11) 0.045(8) Uiso 1 1 d . . . . .
H2B H -0.421(4) 0.325(3) 0.3725(10) 0.034(7) Uiso 1 1 d . . . . .
O3 O -0.14360(19) 0.5449(2) 0.42992(6) 0.0308(3) Uani 1 1 d . . . . .
H3A H -0.048(4) 0.491(4) 0.4382(11) 0.046(8) Uiso 1 1 d . . . . .
H3B H -0.170(5) 0.583(5) 0.4582(16) 0.087(13) Uiso 1 1 d . . . . .
P1 P 0.05923(5) 0.62460(5) 0.31452(2) 0.01614(11) Uani 1 1 d . . . . .
O11 O -0.01479(15) 0.45534(15) 0.31669(5) 0.0195(2) Uani 1 1 d . . . . .
O12 O -0.03486(16) 0.74080(16) 0.35411(5) 0.0234(3) Uani 1 1 d . . . . .
H12 H -0.066(4) 0.684(4) 0.3815(11) 0.047(8) Uiso 1 1 d . . . . .
O13 O 0.05795(15) 0.71942(16) 0.26595(5) 0.0225(3) Uani 1 1 d . . . . .
P2 P 0.58656(5) 0.64039(5) 0.24949(2) 0.01493(11) Uani 1 1 d . . . . .
O21 O 0.41194(15) 0.64425(15) 0.22403(4) 0.0186(2) Uani 1 1 d . . . . .
O22 O 0.66910(15) 0.47337(14) 0.25477(4) 0.0186(2) Uani 1 1 d . . . . .
O23 O 0.71228(17) 0.75931(16) 0.22051(5) 0.0226(3) Uani 1 1 d . . . . .
H23 H 0.816(4) 0.744(4) 0.2274(12) 0.051(8) Uiso 1 1 d . . . . .
S3 S 0.76967(6) 0.74724(5) 0.55835(2) 0.02147(11) Uani 1 1 d . . . . .
O31 O 0.64706(18) 0.73153(19) 0.59900(5) 0.0315(3) Uani 1 1 d . . . . .
O32 O 0.8435(2) 0.58771(19) 0.54346(6) 0.0361(3) Uani 1 1 d . . . . .
O33 O 0.90271(18) 0.87121(18) 0.56761(5) 0.0280(3) Uani 1 1 d . . . . .
N1 N 0.38357(17) 0.76655(17) 0.32602(5) 0.0154(3) Uani 1 1 d . . . . .
H1 H 0.344(3) 0.819(3) 0.3001(9) 0.020(5) Uiso 1 1 d . . . . .
C1 C 0.6481(2) 0.8043(2) 0.50384(6) 0.0211(3) Uani 1 1 d . . . . .
C2 C 0.7200(2) 0.9060(2) 0.46747(7) 0.0227(3) Uani 1 1 d . . . . .
H2 H 0.835(3) 0.956(3) 0.4724(8) 0.027(6) Uiso 1 1 d . . . . .
C3 C 0.6277(2) 0.9321(2) 0.42296(7) 0.0218(3) Uani 1 1 d . . . . .
H3 H 0.676(3) 1.005(3) 0.3988(9) 0.026(6) Uiso 1 1 d . . . . .
C4 C 0.4657(2) 0.8584(2) 0.41471(6) 0.0193(3) Uani 1 1 d . . . . .
C5 C 0.3941(2) 0.7602(2) 0.45210(7) 0.0245(4) Uani 1 1 d . . . . .
H5 H 0.286(3) 0.716(3) 0.4493(10) 0.038(7) Uiso 1 1 d . . . . .
C6 C 0.4852(2) 0.7321(2) 0.49671(7) 0.0251(4) Uani 1 1 d . . . . .
H6 H 0.440(3) 0.663(3) 0.5200(10) 0.037(7) Uiso 1 1 d . . . . .
C7 C 0.3645(2) 0.8946(2) 0.36724(6) 0.0194(3) Uani 1 1 d . . . . .
H7A H 0.240(3) 0.901(3) 0.3742(8) 0.020(5) Uiso 1 1 d . . . . .
H7B H 0.403(3) 0.996(3) 0.3529(8) 0.026(6) Uiso 1 1 d . . . . .
C8 C 0.5696(2) 0.7349(2) 0.31231(6) 0.0179(3) Uani 1 1 d . . . . .
H8A H 0.628(3) 0.836(3) 0.3118(9) 0.024(5) Uiso 1 1 d . . . . .
H8B H 0.619(3) 0.670(3) 0.3365(9) 0.027(6) Uiso 1 1 d . . . . .
C9 C 0.2854(2) 0.6094(2) 0.33514(6) 0.0172(3) Uani 1 1 d . . . . .
H9A H 0.293(3) 0.580(3) 0.3698(9) 0.026(5) Uiso 1 1 d . . . . .
H9B H 0.339(3) 0.522(3) 0.3161(8) 0.019(5) Uiso 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 O1 2.0993(15) . ?
Mg1 O2 2.0681(16) . ?
Mg1 O11 2.0267(13) . ?
Mg1 O13 2.1023(15) 2_545 ?
Mg1 O21 2.0615(13) 2_545 ?
Mg1 O22 2.0714(13) 1_455 ?
P1 O11 1.4846(12) . ?
P1 O12 1.5893(14) . ?
P1 O13 1.5010(13) . ?
P1 C9 1.8144(17) . ?
O13 Mg1 2.1023(15) 2 ?
P2 O21 1.4914(12) . ?
P2 O22 1.4987(12) . ?
P2 O23 1.5691(13) . ?
P2 C8 1.8412(18) . ?
O21 Mg1 2.0615(13) 2 ?
O22 Mg1 2.0714(13) 1_655 ?
S3 O31 1.4438(15) . ?
S3 O32 1.4663(15) . ?
S3 O33 1.4490(14) . ?
S3 C1 1.7733(18) . ?
N1 C7 1.516(2) . ?
N1 C8 1.496(2) . ?
N1 C9 1.499(2) . ?
C1 C2 1.388(3) . ?
C1 C6 1.389(3) . ?
C2 C3 1.387(2) . ?
C3 C4 1.391(2) . ?
C4 C5 1.390(3) . ?
C4 C7 1.501(2) . ?
C5 C6 1.386(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Mg1 O13 86.44(6) . 2_545 ?
O2 Mg1 O1 88.92(7) . . ?
O2 Mg1 O13 174.96(6) . 2_545 ?
O2 Mg1 O22 93.25(6) . 1_455 ?
O11 Mg1 O1 89.71(6) . . ?
O11 Mg1 O2 87.79(6) . . ?
O11 Mg1 O13 90.21(5) . 2_545 ?
O11 Mg1 O21 175.10(6) . 2_545 ?
O11 Mg1 O22 90.63(6) . 1_455 ?
O21 Mg1 O1 94.64(6) 2_545 . ?
O21 Mg1 O2 90.03(6) 2_545 . ?
O21 Mg1 O13 92.31(5) 2_545 2_545 ?
O21 Mg1 O22 85.11(5) 2_545 1_455 ?
O22 Mg1 O1 177.81(6) 1_455 . ?
O22 Mg1 O13 91.40(6) 1_455 2_545 ?
O11 P1 O12 110.19(7) . . ?
O11 P1 O13 120.45(8) . . ?
O11 P1 C9 106.81(7) . . ?
O12 P1 C9 106.17(8) . . ?
O13 P1 O12 105.47(8) . . ?
O13 P1 C9 106.92(8) . . ?
P1 O11 Mg1 149.58(8) . . ?
P1 O13 Mg1 145.68(8) . 2 ?
O21 P2 O22 115.85(7) . . ?
O21 P2 O23 108.44(7) . . ?
O21 P2 C8 109.28(7) . . ?
O22 P2 O23 109.85(7) . . ?
O22 P2 C8 108.92(8) . . ?
O23 P2 C8 103.83(8) . . ?
P2 O21 Mg1 144.77(8) . 2 ?
P2 O22 Mg1 151.81(8) . 1_655 ?
O31 S3 O32 112.32(10) . . ?
O31 S3 O33 113.31(9) . . ?
O31 S3 C1 107.07(8) . . ?
O32 S3 C1 102.11(8) . . ?
O33 S3 O32 112.57(9) . . ?
O33 S3 C1 108.61(8) . . ?
C8 N1 C7 113.11(13) . . ?
C8 N1 C9 111.96(13) . . ?
C9 N1 C7 114.28(13) . . ?
C2 C1 S3 120.94(13) . . ?
C2 C1 C6 121.18(16) . . ?
C6 C1 S3 117.63(14) . . ?
C3 C2 C1 118.76(16) . . ?
C2 C3 C4 120.93(17) . . ?
C3 C4 C7 119.97(16) . . ?
C5 C4 C3 119.39(16) . . ?
C5 C4 C7 120.51(16) . . ?
C6 C5 C4 120.41(17) . . ?
C5 C6 C1 119.30(18) . . ?
C4 C7 N1 114.85(14) . . ?
N1 C8 P2 111.61(11) . . ?
N1 C9 P1 111.84(11) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1A O33 0.89(3) 1.97(3) 2.848(2) 170(3) 3_666
O2 H2A O3 0.85(3) 1.91(3) 2.755(2) 170(3) .
O2 H2B O31 0.78(3) 1.95(3) 2.728(2) 174(3) 3_566
O3 H3A O32 0.88(3) 1.75(3) 2.625(2) 171(3) 3_666
O12 H12 O3 0.89(3) 1.82(3) 2.702(2) 171(3) .
N1 H1 O22 0.86(2) 1.92(2) 2.7477(19) 160(2) 2_655

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
O11 P1 O13 Mg1 -99.49(15) . . . 2 ?
O11 P1 C9 N1 169.90(11) . . . . ?
O12 P1 O11 Mg1 81.74(17) . . . . ?
O12 P1 O13 Mg1 135.20(14) . . . 2 ?
O12 P1 C9 N1 -72.52(13) . . . . ?
O13 P1 O11 Mg1 -41.34(19) . . . . ?
O13 P1 C9 N1 39.72(13) . . . . ?
O21 P2 O22 Mg1 -132.08(15) . . . 1_655 ?
O21 P2 C8 N1 9.38(14) . . . . ?
O22 P2 O21 Mg1 175.87(12) . . . 2 ?
O22 P2 C8 N1 -118.08(12) . . . . ?
O23 P2 O21 Mg1 -60.14(15) . . . 2 ?
O23 P2 O22 Mg1 104.66(17) . . . 1_655 ?
O23 P2 C8 N1 124.92(12) . . . . ?
S3 C1 C2 C3 172.81(14) . . . . ?
S3 C1 C6 C5 -173.35(15) . . . . ?
O31 S3 C1 C2 147.05(15) . . . . ?
O31 S3 C1 C6 -38.63(17) . . . . ?
O32 S3 C1 C2 -94.77(17) . . . . ?
O32 S3 C1 C6 79.55(16) . . . . ?
O33 S3 C1 C2 24.34(18) . . . . ?
O33 S3 C1 C6 -161.33(15) . . . . ?
C1 C2 C3 C4 0.1(3) . . . . ?
C2 C1 C6 C5 1.0(3) . . . . ?
C2 C3 C4 C5 1.3(3) . . . . ?
C2 C3 C4 C7 177.24(16) . . . . ?
C3 C4 C5 C6 -1.7(3) . . . . ?
C3 C4 C7 N1 97.60(19) . . . . ?
C4 C5 C6 C1 0.6(3) . . . . ?
C5 C4 C7 N1 -86.6(2) . . . . ?
C6 C1 C2 C3 -1.3(3) . . . . ?
C7 N1 C8 P2 -159.76(11) . . . . ?
C7 N1 C9 P1 84.52(14) . . . . ?
C7 C4 C5 C6 -177.57(17) . . . . ?
C8 P2 O21 Mg1 52.42(15) . . . 2 ?
C8 P2 O22 Mg1 -8.44(19) . . . 1_655 ?
C8 N1 C7 C4 -55.06(19) . . . . ?
C8 N1 C9 P1 -145.21(11) . . . . ?
C9 P1 O11 Mg1 -163.36(15) . . . . ?
C9 P1 O13 Mg1 22.48(17) . . . 2 ?
C9 N1 C7 C4 74.63(18) . . . . ?
C9 N1 C8 P2 69.38(15) . . . . ?

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

data_baspp
_database_code_depnum_ccdc_archive 'CCDC 1968803'
loop_
_audit_author_name
_audit_author_address
'Stephan Woehlbrandt'
;Institut fuer Anorganische Chemie, Universitaet Kiel
Germany
;
_audit_update_record             
;
2020-02-04 deposited with the CCDC.	2020-02-07 downloaded from the CCDC.
;
_audit_creation_date             2020-01-23
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         '0.25(C72 H88 Ba8 N8 O80 P16 S8), O'
_chemical_formula_sum            'C18 H20 Ba2 N2 O21 P4 S2'
_chemical_formula_weight         1063.04
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
Ba Ba -0.3244 2.2819 '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'
P P 0.1023 0.0942 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           40
_space_group_name_H-M_alt        'A m a 2'
_space_group_name_Hall           'A 2 -2a'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y, z'
'x+1/2, -y, z'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   15.596(3)
_cell_length_b                   24.683(5)
_cell_length_c                   8.7490(17)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3367.9(12)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    20474
_cell_measurement_temperature    170.00
_cell_measurement_theta_max      57.54
_cell_measurement_theta_min      3.3
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.725
_exptl_absorpt_correction_T_max  0.6281
_exptl_absorpt_correction_T_min  0.1468
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-RED and X-SHAPE (STOE, 2008)'
_exptl_crystal_colour            white
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    2.097
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       flake
_exptl_crystal_F_000             2056
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1717
_diffrn_reflns_av_unetI/netI     0.0803
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            20223
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.303
_diffrn_reflns_theta_min         2.104
_diffrn_ambient_temperature      170.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'STOE IPDS-2'
_diffrn_measurement_method       'Omega scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.870
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.984
_reflns_number_gt                3882
_reflns_number_total             4303
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'X-Area (STOE 2007)'
_computing_data_collection       'X-Area (STOE 2007)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2014)'
_refine_diff_density_max         1.503
_refine_diff_density_min         -2.122
_refine_diff_density_rms         0.212
_refine_ls_abs_structure_details 
;
 Flack x determined using 1573 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.02(3)
_refine_ls_extinction_coef       0.0023(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         4303
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0708
_refine_ls_R_factor_gt           0.0662
_refine_ls_restrained_S_all      1.087
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1122P)²+4.4236P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1812
_refine_ls_wR_factor_ref         0.1867
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2.a Ternary CH refined with riding coordinates:
 N1(H1), N2(H2)
2.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C12(H12A,H12B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2A), C3(H3), C6(H6), C7(H7)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.44778(4) 0.24590(2) 0.32093(16) 0.0398(3) Uani 1 1 d . . . . .
O1 O 0.5990(7) 0.2477(3) 0.1528(13) 0.047(2) Uani 1 1 d . . . . .
P1 P 0.5675(2) 0.14133(13) 0.4897(3) 0.0408(6) Uani 1 1 d . . . . .
O11 O 0.5712(5) 0.1975(3) 0.5514(10) 0.0460(17) Uani 1 1 d . . . . .
O12 O 0.5116(6) 0.1357(4) 0.3529(10) 0.051(2) Uani 1 1 d . . . . .
O13 O 0.5441(6) 0.0997(4) 0.6161(12) 0.048(2) Uani 1 1 d . . . . .
P2 P 0.5770(2) 0.36144(12) 0.4898(3) 0.0409(6) Uani 1 1 d . . . . .
O21 O 0.5197(6) 0.3509(4) 0.3581(10) 0.055(2) Uani 1 1 d . . . . .
O22 O 0.6081(6) 0.3129(3) 0.5740(11) 0.053(2) Uani 1 1 d . . . . .
O23 O 0.5384(6) 0.4050(4) 0.5984(12) 0.049(2) Uani 1 1 d . . . . .
S3 S 0.7500 -0.15783(16) 0.4863(4) 0.0391(8) Uani 1 2 d S T P . .
O31 O 0.7500 -0.1797(6) 0.6388(16) 0.083(6) Uani 1 2 d S T P . .
O32 O 0.6755(9) -0.1707(5) 0.407(2) 0.099(5) Uani 1 1 d . . . . .
S4 S 0.7500 0.66445(16) 0.4641(4) 0.0382(8) Uani 1 2 d S T P . .
O41 O 0.7500 0.6908(5) 0.6155(13) 0.041(2) Uani 1 2 d S T P . .
O42 O 0.6722(5) 0.6749(3) 0.3801(11) 0.0452(18) Uani 1 1 d . . . . .
N1 N 0.7500 0.1239(5) 0.5134(14) 0.037(2) Uani 1 2 d S T P . .
H1 H 0.7500 0.1606 0.5621 0.044 Uiso 1 2 calc RS T P . .
N2 N 0.7500 0.3897(5) 0.5043(15) 0.038(2) Uani 1 2 d S T P . .
H2 H 0.7500 0.3521 0.5468 0.046 Uiso 1 2 calc RS T P . .
C1 C 0.7500 -0.0863(7) 0.512(2) 0.040(3) Uani 1 2 d S T P . .
C2 C 0.6731(7) -0.0589(5) 0.5288(14) 0.042(2) Uani 1 1 d . . . . .
H2A H 0.6203 -0.0774 0.5145 0.051 Uiso 1 1 calc R . . . .
C3 C 0.6735(8) -0.0043(5) 0.5666(16) 0.043(2) Uani 1 1 d . . . . .
H3 H 0.6207 0.0144 0.5775 0.051 Uiso 1 1 calc R . . . .
C4 C 0.7500 0.0231(7) 0.5886(19) 0.040(3) Uani 1 2 d S T P . .
C5 C 0.7500 0.5947(7) 0.507(2) 0.038(3) Uani 1 2 d S T P . .
C6 C 0.8275(7) 0.5678(5) 0.5309(14) 0.042(2) Uani 1 1 d . . . . .
H6 H 0.8803 0.5864 0.5174 0.051 Uiso 1 1 calc R . . . .
C7 C 0.8269(8) 0.5140(5) 0.5750(15) 0.043(2) Uani 1 1 d . . . . .
H7 H 0.8797 0.4956 0.5908 0.052 Uiso 1 1 calc R . . . .
C8 C 0.7500 0.4863(7) 0.5967(18) 0.040(3) Uani 1 2 d S T P . .
C9 C 0.7500 0.4276(7) 0.642(2) 0.045(4) Uani 1 2 d S T P . .
H9 H 0.809(9) 0.413(6) 0.705(17) 0.053 Uiso 1 1 d R . . . .
C10 C 0.6704(6) 0.3940(5) 0.4075(13) 0.040(2) Uani 1 1 d . . . . .
H10A H 0.6821 0.3776 0.3064 0.048 Uiso 1 1 calc R . . . .
H10B H 0.6573 0.4328 0.3909 0.048 Uiso 1 1 calc R . . . .
C11 C 0.7500 0.0819(7) 0.639(2) 0.042(4) Uani 1 2 d S T P . .
H11 H 0.697(9) 0.095(6) 0.697(17) 0.050 Uiso 1 1 d R . . . .
C12 C 0.6710(7) 0.1196(5) 0.4138(13) 0.042(2) Uani 1 1 d . . . . .
H12A H 0.6652 0.0812 0.3826 0.051 Uiso 1 1 calc R . . . .
H12B H 0.6820 0.1408 0.3197 0.051 Uiso 1 1 calc R . . . .
O2 O 0.7500 0.2350(6) 0.520(3) 0.071(4) Uani 1 2 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ba1 O1 2.998(12) 6_655 ?
Ba1 O1 2.780(10) . ?
Ba1 O11 2.757(9) 6_654 ?
Ba1 O11 3.034(9) . ?
Ba1 O12 2.910(9) . ?
Ba1 O21 2.843(9) . ?
Ba1 O22 2.745(9) 6_654 ?
Ba1 O32 2.777(11) 2_655 ?
Ba1 O42 2.756(8) 2_665 ?
O1 Ba1 2.998(12) 6_654 ?
P1 O11 1.488(9) . ?
P1 O12 1.487(9) . ?
P1 O13 1.553(10) . ?
P1 C12 1.826(12) . ?
O11 Ba1 2.757(9) 6_655 ?
P2 O21 1.481(9) . ?
P2 O22 1.487(9) . ?
P2 O23 1.555(10) . ?
P2 C10 1.813(11) . ?
O22 Ba1 2.745(9) 6_655 ?
S3 O31 1.439(15) . ?
S3 O32 1.389(11) . ?
S3 O32 1.389(11) 3_655 ?
S3 C1 1.780(18) . ?
O32 Ba1 2.777(11) 2_655 ?
S4 O41 1.475(12) . ?
S4 O42 1.442(9) 3_655 ?
S4 O42 1.442(9) . ?
S4 C5 1.762(18) . ?
O42 Ba1 2.756(8) 2_665 ?
N1 C11 1.51(2) . ?
N1 C12 1.513(12) . ?
N1 C12 1.513(12) 3_655 ?
N2 C9 1.52(2) . ?
N2 C10 1.506(12) . ?
N2 C10 1.506(12) 3_655 ?
C1 C2 1.384(14) 3_655 ?
C1 C2 1.384(14) . ?
C2 C3 1.387(14) . ?
C3 C4 1.386(13) . ?
C4 C3 1.386(13) 3_655 ?
C4 C11 1.52(2) . ?
C5 C6 1.395(13) 3_655 ?
C5 C6 1.395(13) . ?
C6 C7 1.384(16) . ?
C7 C8 1.393(15) . ?
C8 C7 1.393(15) 3_655 ?
C8 C9 1.50(2) . ?

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 135.9(3) . 6_655 ?
O1 Ba1 O11 79.6(3) . . ?
O1 Ba1 O11 62.0(2) 6_655 . ?
O1 Ba1 O12 77.0(2) . . ?
O1 Ba1 O21 73.2(3) . . ?
O11 Ba1 O1 68.3(3) 6_654 . ?
O11 Ba1 O1 140.9(2) 6_654 6_655 ?
O11 Ba1 O11 146.78(14) 6_654 . ?
O11 Ba1 O12 126.4(3) 6_654 . ?
O11 Ba1 O21 71.2(3) 6_654 . ?
O11 Ba1 O32 119.8(4) 6_654 2_655 ?
O12 Ba1 O1 92.3(2) . 6_655 ?
O12 Ba1 O11 49.5(2) . . ?
O21 Ba1 O1 86.4(2) . 6_655 ?
O21 Ba1 O11 91.9(2) . . ?
O21 Ba1 O12 134.9(3) . . ?
O22 Ba1 O1 82.0(3) 6_654 . ?
O22 Ba1 O1 135.5(3) 6_654 6_655 ?
O22 Ba1 O11 63.9(3) 6_654 6_654 ?
O22 Ba1 O11 121.1(2) 6_654 . ?
O22 Ba1 O12 71.9(2) 6_654 . ?
O22 Ba1 O21 134.2(3) 6_654 . ?
O22 Ba1 O32 68.9(4) 6_654 2_655 ?
O22 Ba1 O42 107.9(3) 6_654 2_665 ?
O32 Ba1 O1 66.7(4) 2_655 6_655 ?
O32 Ba1 O1 137.9(3) 2_655 . ?
O32 Ba1 O11 89.8(4) 2_655 . ?
O32 Ba1 O12 65.5(3) 2_655 . ?
O32 Ba1 O21 148.4(3) 2_655 . ?
O42 Ba1 O1 131.6(2) 2_665 . ?
O42 Ba1 O1 67.4(3) 2_665 6_655 ?
O42 Ba1 O11 74.2(3) 2_665 6_654 ?
O42 Ba1 O11 125.9(3) 2_665 . ?
O42 Ba1 O12 151.3(3) 2_665 . ?
O42 Ba1 O21 66.4(3) 2_665 . ?
O42 Ba1 O32 87.3(3) 2_665 2_655 ?
Ba1 O1 Ba1 107.9(3) . 6_654 ?
O11 P1 O13 111.5(6) . . ?
O11 P1 C12 111.8(5) . . ?
O12 P1 O11 113.7(5) . . ?
O12 P1 O13 111.9(6) . . ?
O12 P1 C12 101.4(5) . . ?
O13 P1 C12 105.8(5) . . ?
Ba1 O11 Ba1 107.5(3) 6_655 . ?
P1 O11 Ba1 141.1(5) . 6_655 ?
P1 O11 Ba1 95.8(4) . . ?
P1 O12 Ba1 101.0(4) . . ?
O21 P2 O22 116.1(6) . . ?
O21 P2 O23 111.3(6) . . ?
O21 P2 C10 104.7(5) . . ?
O22 P2 O23 112.4(6) . . ?
O22 P2 C10 107.0(5) . . ?
O23 P2 C10 104.3(5) . . ?
P2 O21 Ba1 119.2(5) . . ?
P2 O22 Ba1 135.4(5) . 6_655 ?
O31 S3 C1 104.7(8) . . ?
O32 S3 O31 112.2(8) 3_655 . ?
O32 S3 O31 112.2(8) . . ?
O32 S3 O32 113.4(16) . 3_655 ?
O32 S3 C1 106.8(6) . . ?
O32 S3 C1 106.8(6) 3_655 . ?
S3 O32 Ba1 150.1(8) . 2_655 ?
O41 S4 C5 103.9(8) . . ?
O42 S4 O41 112.3(4) 3_655 . ?
O42 S4 O41 112.3(4) . . ?
O42 S4 O42 114.6(8) . 3_655 ?
O42 S4 C5 106.4(5) 3_655 . ?
O42 S4 C5 106.4(5) . . ?
S4 O42 Ba1 142.6(5) . 2_665 ?
C11 N1 C12 111.8(8) . 3_655 ?
C11 N1 C12 111.8(8) . . ?
C12 N1 C12 109.1(12) . 3_655 ?
C10 N2 C9 113.6(8) 3_655 . ?
C10 N2 C9 113.6(8) . . ?
C10 N2 C10 111.0(12) 3_655 . ?
C2 C1 S3 119.8(8) 3_655 . ?
C2 C1 S3 119.8(8) . . ?
C2 C1 C2 120.1(16) 3_655 . ?
C1 C2 C3 119.7(12) . . ?
C4 C3 C2 120.8(12) . . ?
C3 C4 C3 118.9(15) . 3_655 ?
C3 C4 C11 120.6(8) 3_655 . ?
C3 C4 C11 120.6(8) . . ?
C6 C5 S4 119.8(8) . . ?
C6 C5 S4 119.8(8) 3_655 . ?
C6 C5 C6 120.2(16) . 3_655 ?
C7 C6 C5 119.5(12) . . ?
C6 C7 C8 121.0(12) . . ?
C7 C8 C7 118.8(17) . 3_655 ?
C7 C8 C9 120.6(9) . . ?
C7 C8 C9 120.6(9) 3_655 . ?
C8 C9 N2 112.5(15) . . ?
N2 C10 P2 114.0(8) . . ?
N1 C11 C4 116.2(14) . . ?
N1 C12 P1 119.3(8) . . ?

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
O11 P1 O12 Ba1 -1.4(6) . . . . ?
O11 P1 C12 N1 52.9(11) . . . . ?
O12 P1 O11 Ba1 1.4(6) . . . . ?
O12 P1 O11 Ba1 128.7(7) . . . 6_655 ?
O12 P1 C12 N1 174.4(9) . . . . ?
O13 P1 O11 Ba1 1.0(10) . . . 6_655 ?
O13 P1 O11 Ba1 -126.3(4) . . . . ?
O13 P1 O12 Ba1 126.0(5) . . . . ?
O13 P1 C12 N1 -68.6(11) . . . . ?
O21 P2 O22 Ba1 -91.3(8) . . . 6_655 ?
O21 P2 C10 N2 -157.9(9) . . . . ?
O22 P2 O21 Ba1 13.2(8) . . . . ?
O22 P2 C10 N2 -34.2(10) . . . . ?
O23 P2 O21 Ba1 -117.0(6) . . . . ?
O23 P2 O22 Ba1 38.4(9) . . . 6_655 ?
O23 P2 C10 N2 85.1(9) . . . . ?
S3 C1 C2 C3 172.5(11) . . . . ?
O31 S3 O32 Ba1 -45(2) . . . 2_655 ?
O31 S3 C1 C2 -87.2(14) . . . . ?
O31 S3 C1 C2 87.2(14) . . . 3_655 ?
O32 S3 O32 Ba1 83(3) 3_655 . . 2_655 ?
O32 S3 C1 C2 -32.0(17) 3_655 . . 3_655 ?
O32 S3 C1 C2 -153.7(15) . . . 3_655 ?
O32 S3 C1 C2 153.7(15) 3_655 . . . ?
O32 S3 C1 C2 32.0(17) . . . . ?
S4 C5 C6 C7 175.4(11) . . . . ?
O41 S4 O42 Ba1 37.7(11) . . . 2_665 ?
O41 S4 C5 C6 -86.8(14) . . . . ?
O41 S4 C5 C6 86.8(14) . . . 3_655 ?
O42 S4 O42 Ba1 -92.0(10) 3_655 . . 2_665 ?
O42 S4 C5 C6 -32.0(16) . . . 3_655 ?
O42 S4 C5 C6 -154.5(13) 3_655 . . 3_655 ?
O42 S4 C5 C6 32.0(16) 3_655 . . . ?
O42 S4 C5 C6 154.5(13) . . . . ?
C1 S3 O32 Ba1 -159(2) . . . 2_655 ?
C1 C2 C3 C4 0(2) . . . . ?
C2 C1 C2 C3 -2(3) 3_655 . . . ?
C2 C3 C4 C3 2(3) . . . 3_655 ?
C2 C3 C4 C11 -176.2(14) . . . . ?
C3 C4 C11 N1 90.7(14) 3_655 . . . ?
C3 C4 C11 N1 -90.7(14) . . . . ?
C5 S4 O42 Ba1 150.8(9) . . . 2_665 ?
C5 C6 C7 C8 -1(2) . . . . ?
C6 C5 C6 C7 2(3) 3_655 . . . ?
C6 C7 C8 C7 -1(2) . . . 3_655 ?
C6 C7 C8 C9 179.0(14) . . . . ?
C7 C8 C9 N2 89.9(13) 3_655 . . . ?
C7 C8 C9 N2 -89.9(13) . . . . ?
C9 N2 C10 P2 -75.8(13) . . . . ?
C10 P2 O21 Ba1 130.9(5) . . . . ?
C10 P2 O22 Ba1 152.3(7) . . . 6_655 ?
C10 N2 C9 C8 -64.1(9) . . . . ?
C10 N2 C9 C8 64.1(9) 3_655 . . . ?
C10 N2 C10 P2 154.7(6) 3_655 . . . ?
C11 N1 C12 P1 72.3(13) . . . . ?
C12 P1 O11 Ba1 115.5(5) . . . . ?
C12 P1 O11 Ba1 -117.2(8) . . . 6_655 ?
C12 P1 O12 Ba1 -121.6(5) . . . . ?
C12 N1 C11 C4 61.3(8) . . . . ?
C12 N1 C11 C4 -61.3(8) 3_655 . . . ?
C12 N1 C12 P1 -163.5(5) 3_655 . . . ?

_olex2_submission_special_instructions 'No special instructions were received'

# start Validation Reply Form
_vrf_PLAT112_baspp               
; 
PROBLEM: ADDSYM Detects New (Pseudo) Symm. Elem         B         96 %Fit  
RESPONSE: Using the ADDSYM algorithm im Platon provided no additional symmetry.
This is supported by the ADDSYM-SHX algorithm in Platon 
which did not change the space group.
Furthermore, a close inspection of the reciprocal space confirmed 
that no symmetry elements were missed.  
;
_vrf_PLAT306_baspp               
; 
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......         O2 Check 
RESPONSE: Hydrogen Atoms could not be located from the fourier map. 
Attaching H-Atoms via a riding model, the H-atom positions were unstable during 
refinement and were thus omitted for the final refinement. 
;
# end Validation Reply Form
####################################################################### 
# 
# 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_cau
_database_code_depnum_ccdc_archive 'CCDC 1968804'
loop_
_audit_author_name
_audit_author_address
'Stephan Woehlbrandt'
;Institut fuer Anorganische Chemie, Universitaet Kiel
Germany
;
_audit_update_record             
;
2020-02-04 deposited with the CCDC.	2020-02-07 downloaded from the CCDC.
;
_audit_creation_date             2020-01-23
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C9 H23 Mg2 N O15 P2 S, 2(H2 O)'
_chemical_formula_sum            'C9 H27 Mg2 N O17 P2 S'
_chemical_formula_weight         563.93
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
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                   18.8531(8)
_cell_length_b                   5.3729(2)
_cell_length_c                   23.7906(10)
_cell_angle_alpha                90
_cell_angle_beta                 113.1800(10)
_cell_angle_gamma                90
_cell_volume                     2215.34(16)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7978
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      27.07
_cell_measurement_theta_min      2.35
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.429
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6825
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.691
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       rod
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0528
_diffrn_reflns_av_unetI/netI     0.0451
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            25674
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.423
_diffrn_reflns_theta_min         2.350
_diffrn_ambient_temperature      294.32
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3763
_reflns_number_total             5014
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_data_collection       'Bruker AXS APEX 3 v2017.3-0'
_computing_cell_refinement       'Bruker AXS APEX 3 v2017.3-0'
_computing_data_reduction        'Bruker AXS APEX 3 v2017.3-0'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.588
_refine_diff_density_min         -1.069
_refine_diff_density_rms         0.100
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         5014
_refine_ls_number_restraints     27
_refine_ls_R_factor_all          0.0788
_refine_ls_R_factor_gt           0.0536
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0670P)²+6.5390P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1343
_refine_ls_wR_factor_ref         0.1474
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H1A,H1B} of O1, {H2A,H2B} of O2, {H5A,H5B} of O5, {H6A,
  H6B} of O6, {H3A,H3B} of O3, {H4A,H4B} of O4, All C(H,H) groups, All N(H)
  groups
 At 1.5 times of:
  {H8C,H8D} of O8, {H7C,H7D} of O7
2. Restrained distances
 H1-N1
 0.95 with sigma of 0.02
 H6A-O6 = H4A-O4 = H5A-O5 = H5B-O5 = H2A-O2 = H2B-O2 = H4B-O4
 0.9 with sigma of 0.02
 O6-H6B = O1-H1B
 0.9 with sigma of 0.02
 Mg2-H5B = Mg2-H5A = Mg1-H1A = Mg1-H1B
 2.6 with sigma of 0.02
 H5B-O8_$1
 2.1 with sigma of 0.02
 H7D-H1B = H7C-H8D = H5B-H8C_$1
 2.1 with sigma of 0.02
 H8C-H5B_$3 = H8D-H5A_$2 = H7C-H8C
 2.2 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
P2 \\sim C9: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
4.a Free rotating group:
 O7(H7C,H7D), O8(H8C,H8D)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
Mg1 Mg 0.42745(6) 1.3520(2) 0.45451(5) 0.0133(2) Uani 1 1 d D . . . .
Mg2 Mg 0.83195(7) -0.0287(2) 0.52461(6) 0.0170(3) Uani 1 1 d D . . . .
O1 O 0.34965(17) 1.4309(6) 0.36526(13) 0.0306(7) Uani 1 1 d D . . . .
H1A H 0.362(3) 1.552(8) 0.3481(12) 0.037 Uiso 1 1 d DR . . . .
H1B H 0.340(2) 1.302(5) 0.3398(10) 0.037 Uiso 1 1 d DR . . . .
O2 O 0.36061(15) 1.0474(5) 0.45083(13) 0.0218(6) Uani 1 1 d D . . . .
H2A H 0.3254(19) 1.090(8) 0.4641(18) 0.026 Uiso 1 1 d DR . . . .
H2B H 0.373(2) 0.893(4) 0.4619(19) 0.026 Uiso 1 1 d DR . . . .
O3 O 0.80352(19) -0.0240(6) 0.42940(14) 0.0330(7) Uani 1 1 d . . . . .
H3A H 0.806(3) 0.096(10) 0.414(2) 0.040 Uiso 1 1 d R . . . .
H3B H 0.825(3) -0.111(10) 0.414(2) 0.040 Uiso 1 1 d R . . . .
O4 O 0.89529(17) -0.3412(5) 0.5368(2) 0.0496(10) Uani 1 1 d D . . . .
H4A H 0.9442(13) -0.344(11) 0.544(3) 0.059 Uiso 1 1 d DR . . . .
H4B H 0.883(3) -0.501(5) 0.531(3) 0.059 Uiso 1 1 d DR . . . .
O5 O 0.8659(2) -0.0028(8) 0.61979(15) 0.0525(10) Uani 1 1 d D . . . .
H5A H 0.858(3) 0.137(6) 0.6336(12) 0.063 Uiso 1 1 d DR . . . .
H5B H 0.854(3) -0.162(5) 0.6328(11) 0.063 Uiso 1 1 d DR . . . .
O6 O 0.93553(15) 0.1470(5) 0.53412(13) 0.0264(6) Uani 1 1 d D . . . .
H6A H 0.9790(16) 0.127(8) 0.5657(14) 0.032 Uiso 1 1 d DR . . . .
H6B H 0.941(3) 0.175(9) 0.4996(13) 0.032 Uiso 1 1 d DR . . . .
O7 O 0.3065(4) 1.0678(11) 0.2742(2) 0.107(2) Uani 1 1 d . . . . .
H7C H 0.2770 0.9747 0.2456 0.160 Uiso 1 1 d DG . . . .
H7D H 0.3486 0.9872 0.2896 0.160 Uiso 1 1 d DG . . . .
O8 O 0.3128(4) 1.0315(15) 0.1557(3) 0.141(3) Uani 1 1 d D . . . .
H8C H 0.3409 0.9519 0.1876 0.212 Uiso 1 1 d DG . . . .
H8D H 0.2883 1.1353 0.1683 0.212 Uiso 1 1 d DG . . . .
P1 P 0.48862(5) 0.86581(16) 0.40512(4) 0.0126(2) Uani 1 1 d . . . . .
O11 O 0.49551(14) 1.1359(4) 0.42350(11) 0.0169(5) Uani 1 1 d . . . . .
O12 O 0.48996(13) 0.6800(4) 0.45478(10) 0.0130(5) Uani 1 1 d . . . . .
O13 O 0.42373(14) 0.8081(5) 0.34467(11) 0.0239(6) Uani 1 1 d . . . . .
P2 P 0.71266(5) 0.48315(15) 0.49731(4) 0.0139(2) Uani 1 1 d . U . . .
O21 O 0.77565(14) 0.2916(5) 0.51865(12) 0.0210(6) Uani 1 1 d . . . . .
O22 O 0.64522(13) 0.4389(4) 0.51556(11) 0.0162(5) Uani 1 1 d . . . . .
O23 O 0.74259(14) 0.7466(4) 0.51279(12) 0.0206(5) Uani 1 1 d . . . . .
S3 S 0.60762(6) 0.96762(19) 0.12160(4) 0.0234(2) Uani 1 1 d . . . . .
O31 O 0.68619(16) 0.9164(6) 0.12875(13) 0.0371(7) Uani 1 1 d . . . . .
O32 O 0.55204(15) 0.8351(6) 0.07001(12) 0.0293(6) Uani 1 1 d . . . . .
O33 O 0.5902(2) 1.2294(6) 0.12001(14) 0.0414(8) Uani 1 1 d . . . . .
N1 N 0.58742(16) 0.5248(5) 0.38740(13) 0.0142(6) Uani 1 1 d D . . . .
H1 H 0.565(2) 0.431(6) 0.4082(16) 0.017 Uiso 1 1 d DR . . . .
C1 C 0.5961(2) 0.8379(7) 0.18610(16) 0.0221(8) Uani 1 1 d . . . . .
C2 C 0.6454(2) 0.6545(8) 0.21990(18) 0.0307(9) Uani 1 1 d . . . . .
H2 H 0.6889 0.6145 0.2125 0.037 Uiso 1 1 calc R . . . .
C3 C 0.6304(3) 0.5302(8) 0.26460(19) 0.0309(9) Uani 1 1 d . . . . .
H3 H 0.6637 0.4058 0.2872 0.037 Uiso 1 1 calc R . . . .
C4 C 0.5656(2) 0.5904(7) 0.27603(16) 0.0214(8) Uani 1 1 d . . . . .
C5 C 0.5177(2) 0.7796(8) 0.24276(17) 0.0266(9) Uani 1 1 d . . . . .
H5 H 0.4749 0.8236 0.2507 0.032 Uiso 1 1 calc R . . . .
C6 C 0.5327(2) 0.9038(8) 0.19797(18) 0.0289(9) Uani 1 1 d . . . . .
H6 H 0.5003 1.0311 0.1759 0.035 Uiso 1 1 calc R . . . .
C7 C 0.5444(2) 0.4453(7) 0.32158(17) 0.0212(8) Uani 1 1 d . . . . .
H7A H 0.488(3) 0.464(8) 0.3121(19) 0.025 Uiso 1 1 d R . . . .
H7B H 0.559(2) 0.275(9) 0.3222(18) 0.025 Uiso 1 1 d R . . . .
C8 C 0.5784(2) 0.7975(6) 0.39669(17) 0.0148(7) Uani 1 1 d . . . . .
H8A H 0.580(2) 0.867(7) 0.3659(19) 0.018 Uiso 1 1 d R . . . .
H8B H 0.621(2) 0.841(7) 0.4327(18) 0.018 Uiso 1 1 d R . . . .
C9 C 0.6708(2) 0.4507(7) 0.41415(17) 0.0195(7) Uani 1 1 d . U . . .
H9A H 0.696(2) 0.543(8) 0.3972(19) 0.023 Uiso 1 1 d R . . . .
H9B H 0.668(2) 0.283(8) 0.4037(18) 0.023 Uiso 1 1 d R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mg1 Mg1 3.168(2) 3_686 ?
Mg1 O1 2.095(3) . ?
Mg1 O2 2.046(3) . ?
Mg1 O11 2.070(2) . ?
Mg1 O12 2.119(2) 1_565 ?
Mg1 O12 2.113(2) 3_676 ?
Mg1 O22 2.101(3) 3_676 ?
Mg2 O3 2.112(3) . ?
Mg2 O4 2.014(3) . ?
Mg2 O5 2.101(3) . ?
Mg2 O6 2.100(3) . ?
Mg2 O21 1.998(3) . ?
Mg2 O23 2.000(3) 1_545 ?
P1 O11 1.506(2) . ?
P1 O12 1.539(2) . ?
P1 O13 1.509(3) . ?
P1 C8 1.818(3) . ?
O12 Mg1 2.113(2) 3_676 ?
O12 Mg1 2.119(2) 1_545 ?
P2 O21 1.501(2) . ?
P2 O22 1.515(2) . ?
P2 O23 1.514(2) . ?
P2 C9 1.827(4) . ?
O22 Mg1 2.101(2) 3_676 ?
O23 Mg2 2.000(3) 1_565 ?
S3 O31 1.449(3) . ?
S3 O32 1.449(3) . ?
S3 O33 1.441(3) . ?
S3 C1 1.775(4) . ?
N1 C7 1.514(5) . ?
N1 C8 1.501(4) . ?
N1 C9 1.498(4) . ?
C1 C2 1.376(5) . ?
C1 C6 1.378(5) . ?
C2 C3 1.375(5) . ?
C3 C4 1.391(5) . ?
C4 C5 1.383(5) . ?
C4 C7 1.511(5) . ?
C5 C6 1.377(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Mg1 Mg1 131.50(10) . 3_686 ?
O1 Mg1 O12 90.08(11) . 1_565 ?
O1 Mg1 O12 172.78(12) . 3_676 ?
O1 Mg1 O22 86.87(12) . 3_676 ?
O2 Mg1 Mg1 141.48(10) . 3_686 ?
O2 Mg1 O1 86.84(12) . . ?
O2 Mg1 O11 89.66(10) . . ?
O2 Mg1 O12 99.93(11) . 3_676 ?
O2 Mg1 O12 176.24(11) . 1_565 ?
O2 Mg1 O22 88.25(10) . 3_676 ?
O11 Mg1 Mg1 92.03(8) . 3_686 ?
O11 Mg1 O1 92.14(12) . . ?
O11 Mg1 O12 92.61(10) . 1_565 ?
O11 Mg1 O12 90.43(10) . 3_676 ?
O11 Mg1 O22 177.73(11) . 3_676 ?
O12 Mg1 Mg1 41.46(6) 1_565 3_686 ?
O12 Mg1 Mg1 41.59(7) 3_676 3_686 ?
O12 Mg1 O12 83.06(10) 3_676 1_565 ?
O22 Mg1 Mg1 90.15(8) 3_676 3_686 ?
O22 Mg1 O12 89.43(10) 3_676 1_565 ?
O22 Mg1 O12 90.80(10) 3_676 3_676 ?
O4 Mg2 O3 92.87(16) . . ?
O4 Mg2 O5 89.33(17) . . ?
O4 Mg2 O6 83.44(12) . . ?
O5 Mg2 O3 174.71(16) . . ?
O6 Mg2 O3 86.72(13) . . ?
O6 Mg2 O5 88.75(15) . . ?
O21 Mg2 O3 90.58(13) . . ?
O21 Mg2 O4 175.43(15) . . ?
O21 Mg2 O5 86.98(14) . . ?
O21 Mg2 O6 93.77(11) . . ?
O21 Mg2 O23 96.63(11) . 1_545 ?
O23 Mg2 O3 90.70(13) 1_545 . ?
O23 Mg2 O4 86.33(12) 1_545 . ?
O23 Mg2 O5 94.24(15) 1_545 . ?
O23 Mg2 O6 169.31(12) 1_545 . ?
O11 P1 O12 115.37(13) . . ?
O11 P1 O13 114.82(15) . . ?
O11 P1 C8 104.40(15) . . ?
O12 P1 C8 102.65(15) . . ?
O13 P1 O12 111.13(14) . . ?
O13 P1 C8 107.11(16) . . ?
P1 O11 Mg1 130.47(14) . . ?
Mg1 O12 Mg1 96.94(10) 3_676 1_545 ?
P1 O12 Mg1 128.27(14) . 3_676 ?
P1 O12 Mg1 134.11(14) . 1_545 ?
O21 P2 O22 115.90(14) . . ?
O21 P2 O23 112.90(14) . . ?
O21 P2 C9 104.36(15) . . ?
O22 P2 C9 103.96(15) . . ?
O23 P2 O22 110.58(13) . . ?
O23 P2 C9 108.27(17) . . ?
P2 O21 Mg2 160.46(17) . . ?
P2 O22 Mg1 138.21(15) . 3_676 ?
P2 O23 Mg2 144.17(15) . 1_565 ?
O31 S3 C1 106.93(18) . . ?
O32 S3 O31 111.77(17) . . ?
O32 S3 C1 104.22(17) . . ?
O33 S3 O31 113.6(2) . . ?
O33 S3 O32 112.09(19) . . ?
O33 S3 C1 107.55(18) . . ?
C8 N1 C7 112.5(3) . . ?
C9 N1 C7 114.2(3) . . ?
C9 N1 C8 111.0(3) . . ?
C2 C1 S3 120.1(3) . . ?
C2 C1 C6 120.3(3) . . ?
C6 C1 S3 119.2(3) . . ?
C3 C2 C1 120.2(4) . . ?
C2 C3 C4 120.1(4) . . ?
C3 C4 C7 121.4(3) . . ?
C5 C4 C3 119.0(3) . . ?
C5 C4 C7 119.5(3) . . ?
C6 C5 C4 120.8(4) . . ?
C5 C6 C1 119.5(4) . . ?
C4 C7 N1 114.2(3) . . ?
N1 C8 P1 112.2(2) . . ?
N1 C9 P2 111.6(2) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1A O13 0.85(4) 1.83(5) 2.615(4) 154(3) 1_565
O1 H1B O7 0.890(18) 1.910(17) 2.789(6) 169(3) .
O2 H2A O23 0.871(19) 1.81(2) 2.662(3) 166(4) 3_676
O2 H2B O22 0.872(19) 1.93(3) 2.747(3) 154(4) 3_666
O3 H3A O31 0.75(5) 2.04(5) 2.786(5) 177(6) 2_645
O4 H4A O32 0.87(2) 1.88(2) 2.742(4) 173(5) 4_666
O4 H4B O6 0.88(2) 2.13(4) 2.860(4) 140(5) 1_545
O4 H4B O21 0.88(2) 2.23(4) 2.898(4) 133(5) 1_545
O6 H6B O32 0.879(19) 1.92(2) 2.769(4) 163(4) 2_645
O7 H7D O13 0.85 1.79 2.594(5) 158.1 .

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

data_PbSPP712B
_database_code_depnum_ccdc_archive 'CCDC 1968805'
loop_
_audit_author_name
_audit_author_address
'Stephan Woehlbrandt'
;Institut fuer Anorganische Chemie, Universitaet Kiel
Germany
;
_audit_update_record             
;
2020-02-04 deposited with the CCDC.	2020-02-07 downloaded from the CCDC.
;
_audit_creation_date             2020-02-04
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
# start Validation Reply Form
_vrf_THETM01_PbSPP712B           
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: The crystal did not diffract to higher angle, even at a
synchrotron source.
;
_vrf_PLAT029_PbSPP712B           
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low
RESPONSE: The beamline only has a single-axis goniometer.
;
_vrf_PLAT084_PbSPP712B           
;
PROBLEM: High wR2 Value (i.e. > 0.25)
RESPONSE: We assign the high R-values to a combination of high disorder in
the crystal and radiation damage from synchrotron radiation.
;
_vrf_PLAT306_PbSPP712B           
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) 
RESPONSE: H-atom orientations did not converge during refinement. 
;
_vrf_PLAT342_PbSPP712B           
;
PROBLEM: Low Bond Precision on C-C Bonds
RESPONSE: We assign the low precision to a combination of high disorder in
the crystal and radiation damage from synchrotron radiation.
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C9 H11 N O9 P2 Pb2 S, 0.5(H2 O)'
_chemical_formula_sum            'C9 H12 N O9.50 P2 Pb2 S'
_chemical_formula_weight         794.58
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0037 0.0017 '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 0.0123 0.0065 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1089 0.1019 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.7576 10.5586 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1294 0.1310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   5.34340(10)
_cell_length_b                   23.6346(3)
_cell_length_c                   13.1707(2)
_cell_angle_alpha                90
_cell_angle_beta                 91.8390(10)
_cell_angle_gamma                90
_cell_volume                     1662.46(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1488
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.894
_cell_measurement_theta_min      1.817
_shelx_estimated_absorpt_T_max   0.898
_shelx_estimated_absorpt_T_min   0.667
_exptl_absorpt_coefficient_mu    22.036
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4380
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1698 before and 0.0791 after correction.
The Ratio of minimum to maximum transmission is 0.5874.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.175
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1436
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.008
_exptl_crystal_size_min          0.005
_exptl_transmission_factor_max   1.0000
_exptl_transmission_factor_min   0.5874
_diffrn_reflns_av_R_equivalents  0.1585
_diffrn_reflns_av_unetI/netI     0.1060
_diffrn_reflns_Laue_measured_fraction_full 0.917
_diffrn_reflns_Laue_measured_fraction_max 0.917
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9995
_diffrn_reflns_point_group_measured_fraction_full 0.917
_diffrn_reflns_point_group_measured_fraction_max 0.917
_diffrn_reflns_theta_full        22.305
_diffrn_reflns_theta_max         22.305
_diffrn_reflns_theta_min         1.817
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.917
_diffrn_measured_fraction_theta_max 0.917
_diffrn_measurement_device       'Biomax (Thunnissen, 2013)'
_diffrn_measurement_device_type  'Eiger 16M detector'
_diffrn_measurement_method       'φ scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.72932
_diffrn_source                   synchrotron
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1206
_reflns_number_total             1804
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'DIALS (Evans, 2018)'
_computing_data_collection       'MXCube3 (Mueller, 2011)'
_computing_data_reduction        
;
DIALS (Evans, 2018)
SADABS (Bruker, 2018)
;
_computing_molecular_graphics    
;
Olex2 (Dolomanov, 2009)
Diamond (Brandenburg, 2014)
;
_computing_publication_material  
;
Encifer (Allen, 2004)
Publcif (Westrip, 2010)
;
_computing_structure_refinement  
;
SHELXL (Sheldrick, 2015b)
Olex2 (Dolomanov, 2009)
;
_computing_structure_solution    
;
SHELXT (Sheldrick, 2015a)
Platon (Spek, 2009)
;
_refine_diff_density_max         4.370
_refine_diff_density_min         -3.240
_refine_diff_density_rms         0.712
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.482
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         1804
_refine_ls_number_restraints     109
_refine_ls_R_factor_all          0.1808
_refine_ls_R_factor_gt           0.1481
_refine_ls_restrained_S_all      1.438
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3646
_refine_ls_wR_factor_ref         0.3900
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 H10B-O4
 1.98 with sigma of 0.0002
3. Uiso/Uaniso restraints and constraints
Uanis(O5) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim
Ueq, Uanis(O1) \\sim Ueq, Uanis(O7) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O10) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.06
4. Rigid body (RIGU) restrains
 C4, C5, C6, C7, C9, C8, C1, C3, C2, N1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: O10(0.5) H10A(0.5) H10B(0.5)
6.a Free rotating group:
 O10(H10A,H10B)
6.b Ternary CH refined with riding coordinates:
 N1(H1)
6.c Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B), C2(H2A,H2B)
6.d Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C8(H8), C9(H9)
6.e Fitted hexagon refined as free rotating group:
 C4(C5,C6,C7,C8,C9)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Pb1 Pb 1.2393(3) 0.22205(11) 0.13838(17) 0.0536(11) Uani 1 1 d . . . . .
Pb2 Pb 1.2373(4) 0.13123(11) 0.44082(18) 0.0553(12) Uani 1 1 d . . . . .
S003 S 0.244(3) 0.6095(8) 0.2686(13) 0.062(5) Uani 1 1 d . . . . .
P2 P 0.729(2) 0.3194(7) 0.0995(13) 0.049(4) Uani 1 1 d . . . . .
P1 P 1.114(2) 0.2757(7) 0.3686(12) 0.048(4) Uani 1 1 d . . . . .
O5 O 0.849(6) 0.2610(15) 0.110(3) 0.044(9) Uani 1 1 d . U . . .
O6 O 0.448(5) 0.3095(14) 0.079(2) 0.036(9) Uani 1 1 d . . . . .
O3 O 1.137(7) 0.2128(18) 0.369(3) 0.060(10) Uani 1 1 d . U . . .
O7 O 0.059(7) 0.5927(19) 0.190(3) 0.064(11) Uani 1 1 d . U . . .
O2 O 1.200(6) 0.3043(16) 0.467(2) 0.045(9) Uani 1 1 d . . . . .
C4 C 0.379(6) 0.5427(11) 0.309(3) 0.044(11) Uani 1 1 d . U . . .
C5 C 0.260(5) 0.4922(14) 0.283(3) 0.075(19) Uani 1 1 d G U . . .
H5 H 0.110181 0.492748 0.244782 0.090 Uiso 1 1 calc R . . . .
C6 C 0.365(6) 0.4409(12) 0.313(3) 0.066(17) Uani 1 1 d G U . . .
H6 H 0.285719 0.407090 0.295380 0.080 Uiso 1 1 calc R . . . .
C7 C 0.589(6) 0.4400(11) 0.370(3) 0.052(11) Uani 1 1 d G U . . .
C8 C 0.708(5) 0.4905(14) 0.396(2) 0.049(12) Uani 1 1 d G U . . .
H8 H 0.857406 0.489917 0.434180 0.059 Uiso 1 1 calc R . . . .
C9 C 0.602(5) 0.5418(11) 0.366(3) 0.045(11) Uani 1 1 d G U . . .
H9 H 0.681872 0.575576 0.383582 0.053 Uiso 1 1 calc R . . . .
O4 O 0.852(6) 0.3601(3) 0.025(2) 0.046(9) Uani 1 1 d D . . . .
O8 O 0.138(7) 0.630(2) 0.357(3) 0.069(13) Uani 1 1 d . . . . .
C1 C 0.779(9) 0.362(2) 0.215(4) 0.038(10) Uani 1 1 d . U . . .
H1A H 0.957809 0.368537 0.224098 0.045 Uiso 1 1 calc R . . . .
H1B H 0.703090 0.399100 0.202231 0.045 Uiso 1 1 calc R . . . .
O9 O 0.437(6) 0.641(2) 0.227(3) 0.067(12) Uani 1 1 d . . . . .
N1 N 0.684(7) 0.341(2) 0.314(3) 0.043(8) Uani 1 1 d . U . . .
H1 H 0.502895 0.336750 0.302536 0.052 Uiso 1 1 calc R . . . .
C3 C 0.710(10) 0.386(2) 0.389(4) 0.048(8) Uani 1 1 d . U . . .
H3A H 0.887163 0.392939 0.400111 0.057 Uiso 1 1 calc R . . . .
H3B H 0.647688 0.371371 0.452513 0.057 Uiso 1 1 calc R . . . .
O1 O 1.233(6) 0.2962(17) 0.276(3) 0.049(9) Uani 1 1 d . U . . .
C2 C 0.768(9) 0.286(2) 0.348(4) 0.044(10) Uani 1 1 d . U . . .
H2A H 0.709018 0.258178 0.298044 0.053 Uiso 1 1 calc R . . . .
H2B H 0.687453 0.277136 0.411050 0.053 Uiso 1 1 calc R . . . .
O10 O 0.780(14) 0.4766(3) 0.038(7) 0.08(3) Uani 0.5 1 d . U P A -1
H10A H 0.843018 0.496540 -0.008777 0.118 Uiso 0.5 1 d G . P A -1
H10B H 0.840939 0.443757 0.029358 0.118 Uiso 0.5 1 d DG . P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 O5 2.30(3) . ?
Pb1 O6 2.49(4) 1_655 ?
Pb1 O2 2.34(4) 4_565 ?
Pb1 O1 2.52(4) . ?
Pb2 O6 2.53(3) 4_666 ?
Pb2 O3 2.21(4) . ?
Pb2 O7 2.48(4) 2_645 ?
Pb2 O4 2.38(3) 4_566 ?
S003 O7 1.46(4) . ?
S003 C4 1.81(3) . ?
S003 O8 1.40(4) . ?
S003 O9 1.40(5) . ?
P2 O5 1.53(4) . ?
P2 O6 1.53(3) . ?
P2 O4 1.54(3) . ?
P2 C1 1.84(5) . ?
P1 O3 1.49(4) . ?
P1 O2 1.52(3) . ?
P1 O1 1.48(4) . ?
P1 C2 1.87(5) . ?
C4 C5 1.3900 . ?
C4 C9 1.3900 . ?
C5 H5 0.9300 . ?
C5 C6 1.3900 . ?
C6 H6 0.9300 . ?
C6 C7 1.3900 . ?
C7 C8 1.3900 . ?
C7 C3 1.45(6) . ?
C8 H8 0.9300 . ?
C8 C9 1.3900 . ?
C9 H9 0.9300 . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 N1 1.51(7) . ?
N1 H1 0.9800 . ?
N1 C3 1.45(7) . ?
N1 C2 1.44(7) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
O10 H10A 0.8507 . ?
O10 H10B 0.8501 . ?

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 Pb1 O6 91.7(11) . 1_655 ?
O5 Pb1 O2 84.2(11) . 4_565 ?
O5 Pb1 O1 78.8(12) . . ?
O6 Pb1 O1 70.5(11) 1_655 . ?
O2 Pb1 O6 86.9(11) 4_565 1_655 ?
O2 Pb1 O1 151.0(13) 4_565 . ?
O3 Pb2 O6 85.5(13) . 4_666 ?
O3 Pb2 O7 83.2(15) . 2_645 ?
O3 Pb2 O4 85.5(11) . 4_566 ?
O7 Pb2 O6 164.4(12) 2_645 4_666 ?
O4 Pb2 O6 89.5(9) 4_566 4_666 ?
O4 Pb2 O7 79.1(11) 4_566 2_645 ?
O7 S003 C4 103(2) . . ?
O8 S003 O7 114(3) . . ?
O8 S003 C4 103(3) . . ?
O9 S003 O7 111(2) . . ?
O9 S003 C4 106(2) . . ?
O9 S003 O8 118(3) . . ?
O5 P2 O6 107(2) . . ?
O5 P2 O4 115.9(18) . . ?
O5 P2 C1 112(2) . . ?
O6 P2 O4 114.6(19) . . ?
O6 P2 C1 110(2) . . ?
O4 P2 C1 98(2) . . ?
O3 P1 O2 115(2) . . ?
O3 P1 C2 102(2) . . ?
O2 P1 C2 110(2) . . ?
O1 P1 O3 107(2) . . ?
O1 P1 O2 115(2) . . ?
O1 P1 C2 107(2) . . ?
P2 O5 Pb1 139(2) . . ?
Pb1 O6 Pb2 119.5(11) 1_455 4_465 ?
P2 O6 Pb1 121.1(18) . 1_455 ?
P2 O6 Pb2 116.9(19) . 4_465 ?
P1 O3 Pb2 153(3) . . ?
S003 O7 Pb2 143(3) . 2_655 ?
P1 O2 Pb1 136(2) . 4_566 ?
C5 C4 S003 120.1(17) . . ?
C5 C4 C9 120.0 . . ?
C9 C4 S003 119.9(17) . . ?
C4 C5 H5 120.0 . . ?
C4 C5 C6 120.0 . . ?
C6 C5 H5 120.0 . . ?
C5 C6 H6 120.0 . . ?
C7 C6 C5 120.0 . . ?
C7 C6 H6 120.0 . . ?
C6 C7 C3 118(3) . . ?
C8 C7 C6 120.0 . . ?
C8 C7 C3 121(3) . . ?
C7 C8 H8 120.0 . . ?
C7 C8 C9 120.0 . . ?
C9 C8 H8 120.0 . . ?
C4 C9 H9 120.0 . . ?
C8 C9 C4 120.0 . . ?
C8 C9 H9 120.0 . . ?
P2 O4 Pb2 138.2(14) . 4_565 ?
P2 C1 H1A 107.5 . . ?
P2 C1 H1B 107.5 . . ?
H1A C1 H1B 107.0 . . ?
N1 C1 P2 119(3) . . ?
N1 C1 H1A 107.5 . . ?
N1 C1 H1B 107.5 . . ?
C1 N1 H1 104.7 . . ?
C3 N1 C1 108(4) . . ?
C3 N1 H1 104.7 . . ?
C2 N1 C1 117(4) . . ?
C2 N1 H1 104.7 . . ?
C2 N1 C3 116(4) . . ?
C7 C3 H3A 107.4 . . ?
C7 C3 H3B 107.4 . . ?
N1 C3 C7 120(5) . . ?
N1 C3 H3A 107.4 . . ?
N1 C3 H3B 107.4 . . ?
H3A C3 H3B 106.9 . . ?
P1 O1 Pb1 112(2) . . ?
P1 C2 H2A 108.0 . . ?
P1 C2 H2B 108.0 . . ?
N1 C2 P1 117(4) . . ?
N1 C2 H2A 108.0 . . ?
N1 C2 H2B 108.0 . . ?
H2A C2 H2B 107.3 . . ?
H10A O10 H10B 104.5 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
