# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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_PhaseII
_database_code_depnum_ccdc_archive 'CCDC 2034999'
loop_
_audit_author_name
_audit_author_address
'Anna Gagor'
;ILT SR PAS Wroclaw Poland
Poland
;
_audit_update_record             
;
2020-12-18 deposited with the CCDC.	2021-02-01 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT112_PhaseII             
;
PROBLEM: ADDSYM Detects New (Pseudo) Symm. Elem         C        100 %Fit
RESPONSE: 1663 peaks with int>3sigma  break the systematic absences for C centring
;

_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            'C H11 Cd N2 O6 P3'
_chemical_formula_weight         352.43

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'
Cd Cd -0.8075 1.2024 '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'

_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                   13.7142(2)
_cell_length_b                   10.3493(3)
_cell_length_c                   7.4175(5)
_cell_angle_alpha                90
_cell_angle_beta                 103.390(4)
_cell_angle_gamma                90
_cell_volume                     1024.16(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    100.00(10)
_cell_measurement_reflns_used    8167
_cell_measurement_theta_min      3.4660
_cell_measurement_theta_max      29.1480

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.286
_exptl_crystal_F_000             688
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    2.602
_exptl_absorpt_correction_T_min  0.77983
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.888
_oxdiff_exptl_absorpt_empirical_full_max 1.196
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature      100.00(10)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_detector_area_resol_mean 10.6249
_diffrn_reflns_number            24121
_diffrn_reflns_av_unetI/netI     0.0184
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.491
_diffrn_reflns_theta_max         26.369
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             2090
_reflns_number_gt                1644
_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 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Diamond Version 3.2k (Crystal Impact GbR)'
_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)+(0.0182P)²+2.2267P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2090
_refine_ls_number_parameters     155
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0274
_refine_ls_wR_factor_ref         0.0574
_refine_ls_wR_factor_gt          0.0544
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_restrained_S_all      1.079
_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
Cd1 Cd 0.75152(2) 0.74634(2) 0.49989(4) 0.01122(8) Uani 1 1 d . . . . .
P1 P 0.50014(6) 0.68584(7) 0.24787(13) 0.01525(17) Uani 1 1 d . . . . .
P2 P 0.73386(6) 0.57390(8) 0.88795(12) 0.01410(19) Uani 1 1 d . . . . .
P3 P 0.76632(6) 0.92064(8) 0.11188(12) 0.01429(19) Uani 1 1 d . . . . .
O1 O 0.59576(19) 0.7580(3) 0.3095(4) 0.0344(8) Uani 1 1 d . . . . .
O2 O 0.40902(18) 0.7678(3) 0.1850(4) 0.0292(6) Uani 1 1 d . . . . .
O3 O 0.68294(16) 0.6443(2) 0.7124(3) 0.0148(5) Uani 1 1 d . . . . .
O4 O 0.77207(19) 0.4402(2) 0.8676(3) 0.0217(6) Uani 1 1 d . . . . .
O5 O 0.81844(16) 0.8517(2) 0.2878(3) 0.0150(5) Uani 1 1 d . . . . .
O6 O 0.72277(18) 1.0517(2) 0.1302(3) 0.0211(6) Uani 1 1 d . . . . .
H1 H 0.696(3) 0.841(3) 0.026(5) 0.025 Uiso 1 1 d . U . . .
H2 H 0.829(3) 0.930(3) 0.003(5) 0.025 Uiso 1 1 d . U . . .
H3 H 0.668(3) 0.567(3) 0.989(5) 0.025 Uiso 1 1 d . U . . .
H4 H 0.806(3) 0.640(3) 0.974(5) 0.025 Uiso 1 1 d . U . . .
H5 H 0.507(3) 0.602(3) 0.124(5) 0.025 Uiso 1 1 d . U . . .
H6 H 0.492(3) 0.608(3) 0.378(5) 0.025 Uiso 1 1 d . U . . .
N1A N 0.9993(2) 0.2572(2) 0.7525(5) 0.0190(6) Uani 0.565(12) 1 d . . P A 1
H1A1 H 1.053401 0.234507 0.721191 0.023 Uiso 0.565(12) 1 calc R U P A 1
H1A2 H 0.960355 0.199389 0.780945 0.023 Uiso 0.565(12) 1 calc R U P A 1
N2A N 1.0313(5) 0.4718(6) 0.7160(8) 0.026(2) Uani 0.565(12) 1 d . . P A 1
H2A1 H 1.086005 0.453203 0.683918 0.031 Uiso 0.565(12) 1 calc R U P A 1
H2A2 H 1.013386 0.551133 0.720633 0.031 Uiso 0.565(12) 1 calc R U P A 1
C1A C 0.9760(7) 0.3807(9) 0.7570(10) 0.015(2) Uani 0.565(12) 1 d . . P A 1
H1A H 0.917153 0.403016 0.791282 0.018 Uiso 0.565(12) 1 calc R U P A 1
N1B N 0.9993(2) 0.2572(2) 0.7525(5) 0.0190(6) Uani 0.435(12) 1 d . . P A 2
H1B1 H 0.944813 0.233836 0.781907 0.023 Uiso 0.435(12) 1 calc R U P A 2
H1B2 H 1.039623 0.199828 0.727653 0.023 Uiso 0.435(12) 1 calc R U P A 2
N2B N 0.9626(7) 0.4700(9) 0.7819(11) 0.032(3) Uani 0.435(12) 1 d . . P A 2
H2B1 H 0.907696 0.449173 0.811605 0.039 Uiso 0.435(12) 1 calc R U P A 2
H2B2 H 0.978483 0.550084 0.776386 0.039 Uiso 0.435(12) 1 calc R U P A 2
C1B C 1.0211(9) 0.3814(14) 0.7456(14) 0.022(3) Uani 0.435(12) 1 d . . P A 2
H1B H 1.080246 0.405329 0.713620 0.026 Uiso 0.435(12) 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
Cd1 O1 2.275(3) . ?
Cd1 O3 2.274(2) . ?
Cd1 O5 2.275(2) . ?
Cd1 O2 2.280(3) 4_676 ?
Cd1 O4 2.289(2) 2_656 ?
Cd1 O6 2.296(2) 2_645 ?
P1 O1 1.486(3) . ?
P1 O2 1.493(3) . ?
P1 H5 1.28(4) . ?
P1 H6 1.28(4) . ?
P2 O4 1.500(2) . ?
P2 O3 1.514(2) . ?
P2 H3 1.30(4) . ?
P2 H4 1.25(4) . ?
P3 O6 1.501(2) . ?
P3 O5 1.513(2) . ?
P3 H1 1.32(4) . ?
P3 H2 1.31(4) . ?
N1A C1A 1.320(10) . ?
N1A H1A1 0.8600 . ?
N1A H1A2 0.8600 . ?
N2A C1A 1.289(13) . ?
N2A H2A1 0.8600 . ?
N2A H2A2 0.8600 . ?
C1A H1A 0.9300 . ?
N1B C1B 1.324(14) . ?
N1B H1B1 0.8600 . ?
N1B H1B2 0.8600 . ?
N2B C1B 1.287(18) . ?
N2B H2B1 0.8600 . ?
N2B H2B2 0.8600 . ?
C1B H1B 0.9300 . ?

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 Cd1 O3 88.59(9) . . ?
O1 Cd1 O5 90.94(9) . . ?
O3 Cd1 O5 178.95(8) . . ?
O1 Cd1 O2 178.59(11) . 4_676 ?
O3 Cd1 O2 92.23(9) . 4_676 ?
O5 Cd1 O2 88.26(9) . 4_676 ?
O1 Cd1 O4 90.81(10) . 2_656 ?
O3 Cd1 O4 89.27(8) . 2_656 ?
O5 Cd1 O4 89.80(8) . 2_656 ?
O2 Cd1 O4 90.35(10) 4_676 2_656 ?
O1 Cd1 O6 89.96(10) . 2_645 ?
O3 Cd1 O6 90.70(8) . 2_645 ?
O5 Cd1 O6 90.24(8) . 2_645 ?
O2 Cd1 O6 88.88(10) 4_676 2_645 ?
O4 Cd1 O6 179.23(10) 2_656 2_645 ?
O1 P1 O2 115.18(15) . . ?
O1 P1 H5 110.7(16) . . ?
O2 P1 H5 111.0(17) . . ?
O1 P1 H6 107.9(17) . . ?
O2 P1 H6 112.5(16) . . ?
H5 P1 H6 98(2) . . ?
O4 P2 O3 117.37(14) . . ?
O4 P2 H3 108.3(16) . . ?
O3 P2 H3 106.1(17) . . ?
O4 P2 H4 107.5(17) . . ?
O3 P2 H4 109.2(17) . . ?
H3 P2 H4 108(2) . . ?
O6 P3 O5 117.79(14) . . ?
O6 P3 H1 110.2(16) . . ?
O5 P3 H1 105.7(16) . . ?
O6 P3 H2 108.7(16) . . ?
O5 P3 H2 108.6(17) . . ?
H1 P3 H2 105(2) . . ?
P1 O1 Cd1 143.03(16) . . ?
P1 O2 Cd1 139.39(16) . 4_575 ?
P2 O3 Cd1 129.58(12) . . ?
P2 O4 Cd1 132.69(13) . 2_646 ?
P3 O5 Cd1 129.53(13) . . ?
P3 O6 Cd1 130.68(13) . 2_655 ?
C1A N1A H1A1 120.0 . . ?
C1A N1A H1A2 120.0 . . ?
H1A1 N1A H1A2 120.0 . . ?
C1A N2A H2A1 120.0 . . ?
C1A N2A H2A2 120.0 . . ?
H2A1 N2A H2A2 120.0 . . ?
N2A C1A N1A 122.9(8) . . ?
N2A C1A H1A 118.5 . . ?
N1A C1A H1A 118.5 . . ?
C1B N1B H1B1 120.0 . . ?
C1B N1B H1B2 120.0 . . ?
H1B1 N1B H1B2 120.0 . . ?
C1B N2B H2B1 120.0 . . ?
C1B N2B H2B2 120.0 . . ?
H2B1 N2B H2B2 120.0 . . ?
N2B C1B N1B 121.8(11) . . ?
N2B C1B H1B 119.1 . . ?
N1B C1B H1B 119.1 . . ?

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
_geom_hbond_publ_flag
N1A^a H1A1^a O5 0.86 1.99 2.820(3) 163.2 3_766 yes
N1A^a H1A2^a O3 0.86 2.06 2.825(3) 148.1 2_646 yes
N2A^a H2A1^a O6 0.86 2.01 2.852(7) 167.5 4_676 yes
N2A^a H2A2^a O1 0.86 2.29 2.966(7) 135.0 4_676 yes
N2A^a H2A2^a O2 0.86 2.34 3.154(7) 159.2 4_676 yes
C1A^a H1A^a O4 0.93 2.22 3.153(9) 175.4 . yes
N1B^b H1B1^b O3 0.86 1.99 2.825(3) 163.0 2_646 yes
N1B^b H1B2^b O5 0.86 2.05 2.820(3) 149.2 3_766 yes
N2B^b H2B1^b O4 0.86 2.00 2.846(9) 167.7 . yes
N2B^b H2B2^b O1 0.86 2.53 3.335(9) 156.0 4_676 yes
N2B^b H2B2^b O2 0.86 2.15 2.859(10) 139.6 4_676 yes
C1B^b H1B^b O6 0.93 2.23 3.156(12) 176.0 4_676 yes

_refine_diff_density_max         0.831
_refine_diff_density_min         -0.605
_refine_diff_density_rms         0.098



_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_PhaseI
_database_code_depnum_ccdc_archive 'CCDC 2035000'
loop_
_audit_author_name
_audit_author_address
'Anna Gagor'
;ILT SR PAS Wroclaw Poland
Poland
;
_audit_update_record             
;
2020-12-18 deposited with the CCDC.	2021-02-01 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            'C H11 Cd N2 O6 P3'
_chemical_formula_weight         352.43

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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

_cell_length_a                   13.6653(4)
_cell_length_b                   10.3708(3)
_cell_length_c                   7.5573(3)
_cell_angle_alpha                90
_cell_angle_beta                 103.058(3)
_cell_angle_gamma                90
_cell_volume                     1043.33(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    7509
_cell_measurement_theta_min      3.4180
_cell_measurement_theta_max      29.3810

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.244
_exptl_crystal_F_000             688
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    2.554
_exptl_absorpt_correction_T_min  0.85339
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.915
_oxdiff_exptl_absorpt_empirical_full_max 1.131
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_ambient_temperature      295(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_detector_area_resol_mean 10.6249
_diffrn_reflns_number            13593
_diffrn_reflns_av_unetI/netI     0.0155
_diffrn_reflns_av_R_equivalents  0.0301
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.490
_diffrn_reflns_theta_max         29.474
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             1384
_reflns_number_gt                1225
_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 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Diamond Version 3.2k (Crystal Impact GbR)'
_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)+(0.0225P)²+1.1927P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.0020(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1384
_refine_ls_number_parameters     81
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0227
_refine_ls_R_factor_gt           0.0184
_refine_ls_wR_factor_ref         0.0458
_refine_ls_wR_factor_gt          0.0433
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_restrained_S_all      1.068
_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
Cd1 Cd 0.750000 0.750000 0.500000 0.01966(8) Uani 1 2 d S . P . .
P2 P 0.73342(5) 0.57462(5) 0.88316(7) 0.03186(14) Uani 1 1 d . . . . .
P1 P 0.500000 0.69026(8) 0.250000 0.03248(18) Uani 1 2 d S T P . .
O2 O 0.68459(11) 0.64541(14) 0.7127(2) 0.0314(3) Uani 1 1 d . . . . .
O3 O 0.77218(13) 0.44211(14) 0.8658(2) 0.0398(4) Uani 1 1 d . . . . .
O1 O 0.59029(14) 0.76726(18) 0.3300(3) 0.0552(6) Uani 1 1 d . . . . .
N1 N 0.500000 0.7561(2) 0.750000 0.0416(7) Uani 1 2 d S T P . .
H1A H 0.553528 0.732352 0.717128 0.050 Uiso 0.5 1 calc R U P . .
H1B H 0.460047 0.699203 0.777252 0.050 Uiso 0.5 1 calc R U P . .
N2 N 0.5371(4) 0.9658(5) 0.7190(8) 0.0666(16) Uani 0.5 1 d . . P . .
H2A H 0.591075 0.944233 0.685752 0.080 Uiso 0.5 1 calc R U P . .
H2B H 0.522065 1.045862 0.725548 0.080 Uiso 0.5 1 calc R U P . .
H3 H 0.670(3) 0.571(3) 0.988(5) 0.080 Uiso 1 1 d . U . . .
H1 H 0.484(3) 0.611(3) 0.363(4) 0.080 Uiso 1 1 d . U . . .
H2 H 0.809(3) 0.650(3) 0.970(5) 0.080 Uiso 1 1 d . U . . .
C1 C 0.4794(4) 0.8787(5) 0.7585(10) 0.0406(13) Uani 0.5 1 d . . P . .
H1C H 0.421262 0.903172 0.794274 0.049 Uiso 0.5 1 calc R U P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 O1 2.2756(18) . ?
Cd1 O1 2.2757(18) 7_666 ?
Cd1 O2 2.2820(13) . ?
Cd1 O2 2.2820(13) 7_666 ?
Cd1 O3 2.2867(14) 6_565 ?
Cd1 O3 2.2867(14) 4_656 ?
P2 O3 1.4893(15) . ?
P2 O2 1.5020(15) . ?
P2 H3 1.30(4) . ?
P2 H2 1.35(4) . ?
P1 O1 1.4794(18) 2_655 ?
P1 O1 1.4794(18) . ?
P1 H1 1.24(3) . ?
P1 H1 1.24(3) 2_655 ?
N1 C1 1.307(5) . ?
N1 H1A 0.8600 . ?
N1 H1B 0.8600 . ?
N2 C1 1.279(6) . ?
N2 H2A 0.8600 . ?
N2 H2B 0.8600 . ?
C1 H1C 0.9300 . ?

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 Cd1 O1 180.00(9) . 7_666 ?
O1 Cd1 O2 87.51(7) . . ?
O1 Cd1 O2 92.49(7) 7_666 . ?
O1 Cd1 O2 92.49(7) . 7_666 ?
O1 Cd1 O2 87.51(7) 7_666 7_666 ?
O2 Cd1 O2 180.0 . 7_666 ?
O1 Cd1 O3 91.40(7) . 6_565 ?
O1 Cd1 O3 88.60(7) 7_666 6_565 ?
O2 Cd1 O3 90.61(5) . 6_565 ?
O2 Cd1 O3 89.39(5) 7_666 6_565 ?
O1 Cd1 O3 88.60(7) . 4_656 ?
O1 Cd1 O3 91.40(7) 7_666 4_656 ?
O2 Cd1 O3 89.39(5) . 4_656 ?
O2 Cd1 O3 90.61(5) 7_666 4_656 ?
O3 Cd1 O3 180.00(9) 6_565 4_656 ?
O3 P2 O2 118.25(9) . . ?
O3 P2 H3 109.0(14) . . ?
O2 P2 H3 107.9(16) . . ?
O3 P2 H2 109.3(15) . . ?
O2 P2 H2 106.0(15) . . ?
H3 P2 H2 106(2) . . ?
O1 P1 O1 114.66(15) 2_655 . ?
O1 P1 H1 112.1(17) 2_655 . ?
O1 P1 H1 110.0(16) . . ?
O1 P1 H1 110.0(16) 2_655 2_655 ?
O1 P1 H1 112.1(17) . 2_655 ?
H1 P1 H1 97(3) . 2_655 ?
P2 O2 Cd1 131.89(9) . . ?
P2 O3 Cd1 132.80(9) . 4_646 ?
P1 O1 Cd1 142.49(11) . . ?
C1 N1 H1A 120.0 . . ?
C1 N1 H1B 120.0 . . ?
H1A N1 H1B 120.0 . . ?
C1 N2 H2A 120.0 . . ?
C1 N2 H2B 120.0 . . ?
H2A N2 H2B 120.0 . . ?
N2 C1 N1 121.6(4) . . ?
N2 C1 H1C 119.2 . . ?
N1 C1 H1C 119.2 . . ?

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
_geom_hbond_publ_flag
N1 H1A O2 0.86 2.01 2.8429(17) 162.1 . yes
N1 H1B O2 0.86 2.07 2.8429(17) 148.9 2_656 yes
N2 H2A O3 0.86 1.99 2.831(5) 164.4 4_656 yes
N2 H2B O1 0.86 2.45 3.247(5) 154.6 5_676 yes
N2 H2B O1 0.86 2.22 2.936(5) 141.1 6_576 yes
C1 H1C O3 0.93 2.26 3.185(4) 173.5 3_455 yes

_refine_diff_density_max         0.410
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.080



