# Electronic Supplementary Material (ESI) for RSC Advances.
# 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_III
_database_code_depnum_ccdc_archive 'CCDC 1989064'
loop_
_audit_author_name
_audit_author_address
'Anna Gagor'
;ILT SR PAS Wroclaw Poland
Poland
;
_audit_update_record             
;
2020-03-09 deposited with the CCDC.	2020-05-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C1.17 H12.84 Mn N2 O6 P2.83'
_chemical_formula_weight         293.60

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

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

_cell_length_a                   9.3938(6)
_cell_length_b                   13.3012(8)
_cell_length_c                   8.5716(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1071.01(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    3151
_cell_measurement_theta_min      2.8060
_cell_measurement_theta_max      29.1630

_exptl_crystal_description       prism
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.821
_exptl_crystal_F_000             604
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.11
_exptl_absorpt_coefficient_mu    1.657
_diffrn_ambient_temperature      295(2)
_exptl_absorpt_correction_T_min  0.96807
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.971
_oxdiff_exptl_absorpt_empirical_full_max 1.050
_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_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_detector_area_resol_mean 10.6249
_diffrn_reflns_number            6102
_diffrn_reflns_av_unetI/netI     0.0202
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.827
_diffrn_reflns_theta_max         29.506
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.904
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.904
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.904
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             1399
_reflns_number_gt                1111
_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 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0471P)²+1.8779P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1399
_refine_ls_number_parameters     68
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0369
_refine_ls_wR_factor_ref         0.1063
_refine_ls_wR_factor_gt          0.0970
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_restrained_S_all      1.095
_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
Mn1 Mn 0.500000 0.500000 0.500000 0.02288(18) Uani 1 2 d S . P . .
P1 P 0.48975(12) 0.750000 0.64821(12) 0.0323(3) Uani 1 2 d S T P . .
H1A H 0.587670 0.750000 0.684129 0.039 Uiso 1 2 calc R U P . .
H1B H 0.429515 0.750000 0.740127 0.039 Uiso 1 2 calc R U P . .
P2 P 0.18161(11) 0.51581(6) 0.67037(12) 0.0446(3) Uani 0.915 1 d . . P . .
H2A H 0.121998 0.553198 0.598454 0.054 Uiso 0.96 1 calc R U P . .
H2B H 0.231845 0.564449 0.734227 0.054 Uiso 0.96 1 calc R U P . .
C2 C 0.18161(11) 0.51581(6) 0.67037(12) 0.0446(3) Uani 0.085 1 d . . P . .
O1 O 0.0881(2) 0.45627(14) 0.7731(2) 0.0392(5) Uani 1 1 d . . . . .
O2 O 0.2875(2) 0.45972(15) 0.5787(3) 0.0410(5) Uani 1 1 d . . . . .
O3 O 0.4649(3) 0.65533(15) 0.5638(3) 0.0499(6) Uani 1 1 d . . . . .
N2 N 0.1778(3) 0.250000 0.7634(4) 0.0316(7) Uani 1 2 d S T P . .
HB H 0.131327 0.196068 0.797819 0.038 Uiso 0.5 1 calc R U P . .
HC H 0.131327 0.303932 0.797820 0.038 Uiso 0.5 1 calc R U P . .
N1 N 0.1726(4) 0.250000 0.5951(4) 0.0415(9) Uani 1 2 d S T P . .
HA H 0.218763 0.198898 0.558596 0.050 Uiso 1 1 d R U . . .
C1 C 0.3209(5) 0.250000 0.8328(5) 0.0429(10) Uani 1 2 d S T P . .
HD H 0.372054 0.191608 0.798360 0.064 Uiso 0.5 1 calc R U P . .
HE H 0.313039 0.248938 0.944484 0.064 Uiso 0.5 2 calc R U P . .
HF H 0.371000 0.309453 0.800970 0.064 Uiso 0.5 1 calc R U P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mn1 0.0242(3) 0.0149(3) 0.0295(3) 0.00079(19) -0.0008(2) -0.00061(19)
P1 0.0453(6) 0.0170(4) 0.0345(5) 0.000 -0.0041(4) 0.000
P2 0.0540(6) 0.0252(4) 0.0545(6) 0.0044(3) 0.0252(5) 0.0019(4)
C2 0.0540(6) 0.0252(4) 0.0545(6) 0.0044(3) 0.0252(5) 0.0019(4)
O1 0.0492(13) 0.0295(9) 0.0390(11) -0.0034(8) 0.0160(10) -0.0051(9)
O2 0.0359(11) 0.0329(10) 0.0543(13) -0.0054(10) 0.0138(10) -0.0067(9)
O3 0.0652(15) 0.0192(9) 0.0652(15) -0.0099(10) -0.0040(12) 0.0031(10)
N2 0.0279(16) 0.0269(14) 0.0402(18) 0.000 0.0042(14) 0.000
N1 0.056(2) 0.0287(16) 0.0395(19) 0.000 0.0039(17) 0.000
C1 0.032(2) 0.042(2) 0.054(3) 0.000 0.002(2) 0.000

_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
Mn1 O3 2.163(2) 5_666 ?
Mn1 O3 2.163(2) . ?
Mn1 O2 2.174(2) 5_666 ?
Mn1 O2 2.174(2) . ?
Mn1 O1 2.1919(19) 6_657 ?
Mn1 O1 2.1919(19) 2_564 ?
P1 O3 1.471(2) . ?
P1 O3 1.471(2) 7_575 ?
P1 H1A 0.9700 . ?
P1 H1B 0.9700 . ?
P2 O2 1.471(2) . ?
P2 O1 1.475(2) . ?
P2 H2A 0.9700 . ?
P2 H2B 0.9700 . ?
N2 N1 1.443(5) . ?
N2 C1 1.470(5) . ?
N2 HB 0.8900 . ?
N2 HC 0.8900 . ?
N1 HA 0.8651 . ?
N1 HA 0.87(3) 7_565 ?
C1 HD 0.9600 . ?
C1 HE 0.9600 . ?
C1 HF 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Mn1 O3 180.0 5_666 . ?
O3 Mn1 O2 90.97(8) 5_666 5_666 ?
O3 Mn1 O2 89.03(9) . 5_666 ?
O3 Mn1 O2 89.04(9) 5_666 . ?
O3 Mn1 O2 90.96(8) . . ?
O2 Mn1 O2 180.0 5_666 . ?
O3 Mn1 O1 85.01(8) 5_666 6_657 ?
O3 Mn1 O1 94.98(8) . 6_657 ?
O2 Mn1 O1 89.65(9) 5_666 6_657 ?
O2 Mn1 O1 90.35(9) . 6_657 ?
O3 Mn1 O1 94.99(8) 5_666 2_564 ?
O3 Mn1 O1 85.02(8) . 2_564 ?
O2 Mn1 O1 90.35(9) 5_666 2_564 ?
O2 Mn1 O1 89.65(9) . 2_564 ?
O1 Mn1 O1 180.0 6_657 2_564 ?
O3 P1 O3 117.7(2) . 7_575 ?
O3 P1 H1A 107.9 . . ?
O3 P1 H1A 107.9 7_575 . ?
O3 P1 H1B 107.9 . . ?
O3 P1 H1B 107.9 7_575 . ?
H1A P1 H1B 107.2 . . ?
O2 P2 O1 116.72(12) . . ?
O2 P2 H2A 108.1 . . ?
O1 P2 H2A 108.1 . . ?
O2 P2 H2B 108.1 . . ?
O1 P2 H2B 108.1 . . ?
H2A P2 H2B 107.3 . . ?
P2 O1 Mn1 127.76(11) . 2_565 ?
P2 O2 Mn1 131.42(12) . . ?
P1 O3 Mn1 156.62(16) . . ?
N1 N2 C1 115.8(3) . . ?
N1 N2 HB 108.3 . . ?
C1 N2 HB 108.3 . . ?
N1 N2 HC 108.3 . . ?
C1 N2 HC 108.3 . . ?
HB N2 HC 107.4 . . ?
N2 N1 HA 110.2 . . ?
N2 N1 HA 110.2(7) . 7_565 ?
HA N1 HA 103.6 . 7_565 ?
N2 C1 HD 109.5 . . ?
N2 C1 HE 109.5 . . ?
HD C1 HE 109.5 . . ?
N2 C1 HF 109.5 . . ?
HD C1 HF 109.5 . . ?
HE C1 HF 109.5 . . ?

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
N2 HB O1 0.89 2.08 2.871(2) 148.0 7_565 yes
N2 HB O3 0.89 2.51 3.164(4) 130.6 8_656 yes
N2 HC O1 0.89 2.08 2.871(2) 148.0 . yes
N2 HC O3 0.89 2.51 3.164(4) 130.6 2_565 yes
N1 HA O2 0.87 2.21 2.994(2) 150.1 7_565 yes

_refine_diff_density_max         0.344
_refine_diff_density_min         -0.662
_refine_diff_density_rms         0.085

_shelx_res_file                  
;
TITL mhyd_mn_po2_30m_a.res in Pnma
    rt.res
    created by SHELXL-2018/3 at 12:04:27 on 02-Mar-2020
REM Old TITL MHyd_Mn_PO2_30m in Pnma
REM SHELXT solution in Pnma
REM R1 0.121, Rweak 0.143, Alpha 0.033, Orientation as input

CELL 0.71073   9.393833  13.301213   8.571560  90 90 90
ZERR 4 0.000586 0.00076 0.000608 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,-Z
SYMM 0.5+X,0.5-Y,0.5-Z
SFAC H N O P Mn C
UNIT 51.36 8 24 11.32 4 4.68
L.S. 10 0 0
PLAN  20
BOND $H
list 4
fmap 2 53

ACTA
bond $H
htab
omit 4 2 1
omit 0 5 1
EQIV $6 x, -y+1/2, z
HTAB N2 O1_$6
EQIV $7 -x+1/2, y-1/2, z+1/2
HTAB N2 O3_$7
HTAB N2 O1
EQIV $1 -x+1/2, -y+1, z+1/2
HTAB N2 O3_$1
HTAB N1 O2_$6
eadp p2 c2
exyz p2 c2

WGHT    0.046900    0.966800
FVAR       3.76743
MN1   5    0.500000    0.500000    0.500000    10.50000    0.02421    0.01488 =
         0.02955    0.00079   -0.00084   -0.00061
P1    4    0.489750    0.750000    0.648211    10.50000    0.04530    0.01701 =
         0.03448    0.00000   -0.00408    0.00000
AFIX  23
H1A   1    0.587670    0.750000    0.684129    10.50000   -1.20000
H1B   1    0.429515    0.750000    0.740127    10.50000   -1.20000
AFIX   0
P2    4    0.181612    0.515808    0.670367    10.91500    0.05403    0.02521 =
         0.05452    0.00440    0.02517    0.00194
AFIX  23
H2A   1    0.121998    0.553198    0.598454    10.96000   -1.20000
H2B   1    0.231845    0.564449    0.734227    10.96000   -1.20000
AFIX   0

C2    6    0.181612    0.515808    0.670367    10.08500    0.05403    0.02521 =
         0.05452    0.00440    0.02517    0.00194
O1    3    0.088082    0.456274    0.773131    11.00000    0.04920    0.02950 =
         0.03904   -0.00342    0.01604   -0.00506
O2    3    0.287472    0.459723    0.578692    11.00000    0.03589    0.03293 =
         0.05433   -0.00536    0.01380   -0.00667
O3    3    0.464858    0.655335    0.563773    11.00000    0.06521    0.01922 =
         0.06522   -0.00990   -0.00397    0.00314
N2    2    0.177798    0.250000    0.763422    10.50000    0.02793    0.02686 =
         0.04016    0.00000    0.00419    0.00000
AFIX  23
HB    1    0.131327    0.196068    0.797819    10.50000   -1.20000
HC    1    0.131327    0.303932    0.797820    10.50000   -1.20000
AFIX   0
N1    2    0.172583    0.250000    0.595150    10.50000    0.05629    0.02871 =
         0.03951    0.00000    0.00387    0.00000
AFIX   7
HA    1    0.218763    0.198898    0.558596    11.00000   -1.20000
AFIX   0
C1    6    0.320881    0.250000    0.832828    10.50000    0.03227    0.04224 =
         0.05429    0.00000    0.00178    0.00000
AFIX 133
HD    1    0.372054    0.191608    0.798360    10.50000   -1.50000
HE    1    0.313039    0.248938    0.944484    10.50000   -1.50000
HF    1    0.371000    0.309453    0.800970    10.50000   -1.50000

AFIX   0
HKLF 4




REM  mhyd_mn_po2_30m_a.res in Pnma
REM wR2 = 0.1063, GooF = S = 1.095, Restrained GooF = 1.095 for all data
REM R1 = 0.0369 for 1111 Fo > 4sig(Fo) and 0.0497 for all 1399 data
REM 68 parameters refined using 0 restraints

END

WGHT      0.0474      0.9735

REM Instructions for potential hydrogen bonds
HTAB N2 O1_$6
HTAB N2 O3_$7
HTAB N2 O1
HTAB N2 O3_$1
HTAB N1 O2_$6

REM Highest difference peak  0.344,  deepest hole -0.662,  1-sigma level  0.085
Q1    1   0.0063  0.2500  0.8506  10.50000  0.05    0.34
Q2    1   0.2524  0.5904  0.7653  11.00000  0.05    0.32
Q3    1   0.4946  0.6570  0.4990  11.00000  0.05    0.30
Q4    1   0.3440  0.7500  0.7792  10.50000  0.05    0.30
Q5    1   0.4234  0.6567  0.5460  11.00000  0.05    0.29
Q6    1   0.5461  0.6538  0.5742  11.00000  0.05    0.25
Q7    1   0.2742  0.4555  0.6624  11.00000  0.05    0.24
Q8    1   0.3346  0.5569  0.7987  11.00000  0.05    0.24
Q9    1   0.1526  0.4932  0.5979  11.00000  0.05    0.24
Q10   1   0.5130  0.7500  0.8001  10.50000  0.05    0.24
Q11   1   0.0889  0.5786  0.5784  11.00000  0.05    0.24
Q12   1   0.1001  0.5594  0.4695  11.00000  0.05    0.23
Q13   1   0.2834  0.6598  0.7412  11.00000  0.05    0.23
Q14   1   0.6529  0.7500  0.7507  10.50000  0.05    0.23
Q15   1   0.1585  0.6055  0.6700  11.00000  0.05    0.22
Q16   1   0.0486  0.1388  0.7174  11.00000  0.05    0.22
Q17   1   0.4600  0.6464  0.6226  11.00000  0.05    0.22
Q18   1   0.1801  0.5433  0.6770  11.00000  0.05    0.22
Q19   1   0.0733  0.3802  0.7022  11.00000  0.05    0.21
Q20   1   0.3597  0.3341  0.8079  11.00000  0.05    0.21
;
_shelx_res_checksum              48410
####################################################################### 
# 
# 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_II
_database_code_depnum_ccdc_archive 'CCDC 1989066'
loop_
_audit_author_name
_audit_author_address
'Anna Gagor'
;ILT SR PAS Wroclaw Poland
Poland
;
_audit_update_record             
;
2020-03-09 deposited with the CCDC.	2020-05-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C H13 Mn N2 O6 P3'
_chemical_formula_weight         296.98

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

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

_cell_length_a                   9.2009(6)
_cell_length_b                   13.2604(8)
_cell_length_c                   8.5408(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1042.04(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    100.0(2)
_cell_measurement_reflns_used    5364
_cell_measurement_theta_min      2.8360
_cell_measurement_theta_max      29.2010

_exptl_crystal_description       prism
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.893
_exptl_crystal_F_000             604
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.09
_exptl_absorpt_coefficient_mu    1.729
_exptl_absorpt_correction_T_min  0.63799
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.847
_oxdiff_exptl_absorpt_empirical_full_max 1.368
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature      100.0(2)
_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            11095
_diffrn_reflns_av_unetI/netI     0.0169
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.837
_diffrn_reflns_theta_max         25.673
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1037
_reflns_number_gt                1014
_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 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0369P)²+1.7075P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       ?
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1037
_refine_ls_number_parameters     68
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0284
_refine_ls_wR_factor_ref         0.0829
_refine_ls_wR_factor_gt          0.0825
_refine_ls_goodness_of_fit_ref   1.183
_refine_ls_restrained_S_all      1.183
_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
Mn1 Mn 0.500000 0.500000 0.500000 0.0116(2) Uani 1 2 d S . P . .
P1 P 0.49000(9) 0.750000 0.65050(11) 0.0147(3) Uani 1 2 d S T P . .
H1A H 0.591560 0.750001 0.680953 0.018 Uiso 1 2 calc R U P . .
H1B H 0.432834 0.750000 0.745925 0.018 Uiso 1 2 calc R U P . .
P2 P 0.17377(7) 0.51645(5) 0.66490(8) 0.0174(2) Uani 1 1 d . . . . .
H2A H 0.113083 0.557074 0.596729 0.021 Uiso 1 1 calc R U . . .
H2B H 0.228395 0.562375 0.730860 0.021 Uiso 1 1 calc R U . . .
O1 O 0.07619(17) 0.45438(12) 0.7682(2) 0.0169(4) Uani 1 1 d . . . . .
O2 O 0.27933(17) 0.45928(12) 0.5650(2) 0.0174(4) Uani 1 1 d . . . . .
O3 O 0.4600(2) 0.65447(13) 0.5654(2) 0.0221(4) Uani 1 1 d . . . . .
N2 N 0.1705(3) 0.250000 0.7623(4) 0.0152(6) Uani 1 2 d S T P . .
HB H 0.123156 0.195890 0.796942 0.018 Uiso 0.5 1 calc R U P . .
HC H 0.123156 0.304110 0.796942 0.018 Uiso 0.5 1 calc R U P . .
N1 N 0.1651(3) 0.250000 0.5934(4) 0.0181(6) Uani 1 2 d S T P . .
HA H 0.212481 0.199570 0.555645 0.022 Uiso 1 1 d R U . . .
C1 C 0.3187(4) 0.250000 0.8320(5) 0.0187(8) Uani 1 2 d S T P . .
HD H 0.370645 0.191246 0.797540 0.028 Uiso 0.5 1 calc R U P . .
HE H 0.311276 0.249292 0.944095 0.028 Uiso 0.5 2 calc R U P . .
HF H 0.369938 0.309462 0.799284 0.028 Uiso 0.5 1 calc R U P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mn1 0.0067(3) 0.0048(3) 0.0232(4) -0.00010(18) -0.00041(18) -0.00014(16)
P1 0.0115(4) 0.0073(4) 0.0253(5) 0.000 -0.0012(3) 0.000
P2 0.0152(4) 0.0080(3) 0.0290(4) 0.0007(2) 0.0056(3) 0.0002(2)
O1 0.0133(8) 0.0110(8) 0.0265(10) -0.0008(7) 0.0041(7) -0.0017(6)
O2 0.0107(8) 0.0127(8) 0.0287(9) -0.0022(7) 0.0034(7) -0.0036(7)
O3 0.0210(9) 0.0079(8) 0.0374(11) -0.0031(7) -0.0029(8) 0.0017(7)
N2 0.0081(13) 0.0089(13) 0.0285(16) 0.000 0.0014(11) 0.000
N1 0.0189(15) 0.0089(13) 0.0265(16) 0.000 0.0019(13) 0.000
C1 0.0092(16) 0.0145(17) 0.032(2) 0.000 -0.0014(14) 0.000

_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
Mn1 O3 2.1548(17) 5_666 ?
Mn1 O3 2.1548(17) . ?
Mn1 O2 2.1731(16) 5_666 ?
Mn1 O2 2.1731(16) . ?
Mn1 O1 2.1859(17) 6_657 ?
Mn1 O1 2.1859(17) 2_564 ?
P1 O3 1.4863(18) . ?
P1 O3 1.4864(18) 7_575 ?
P1 H1A 0.9700 . ?
P1 H1B 0.9700 . ?
P2 O2 1.4986(18) . ?
P2 O1 1.5037(17) . ?
P2 H2A 0.9700 . ?
P2 H2B 0.9700 . ?
N2 N1 1.444(4) . ?
N2 C1 1.488(4) . ?
N2 HB 0.8900 . ?
N2 HC 0.8900 . ?
N1 HA 0.8609 . ?
N1 HA 0.86(3) 7_565 ?
C1 HD 0.9600 . ?
C1 HE 0.9600 . ?
C1 HF 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Mn1 O3 180.0 5_666 . ?
O3 Mn1 O2 90.59(7) 5_666 5_666 ?
O3 Mn1 O2 89.41(7) . 5_666 ?
O3 Mn1 O2 89.41(7) 5_666 . ?
O3 Mn1 O2 90.59(7) . . ?
O2 Mn1 O2 180.0 5_666 . ?
O3 Mn1 O1 85.24(7) 5_666 6_657 ?
O3 Mn1 O1 94.76(7) . 6_657 ?
O2 Mn1 O1 90.03(7) 5_666 6_657 ?
O2 Mn1 O1 89.97(7) . 6_657 ?
O3 Mn1 O1 94.76(7) 5_666 2_564 ?
O3 Mn1 O1 85.24(7) . 2_564 ?
O2 Mn1 O1 89.97(7) 5_666 2_564 ?
O2 Mn1 O1 90.03(7) . 2_564 ?
O1 Mn1 O1 180.0 6_657 2_564 ?
O3 P1 O3 116.93(16) . 7_575 ?
O3 P1 H1A 108.1 . . ?
O3 P1 H1A 108.1 7_575 . ?
O3 P1 H1B 108.1 . . ?
O3 P1 H1B 108.1 7_575 . ?
O2 P2 O1 116.36(10) . . ?
O2 P2 H2A 108.2 . . ?
O1 P2 H2A 108.2 . . ?
O2 P2 H2B 108.2 . . ?
O1 P2 H2B 108.2 . . ?
P2 O1 Mn1 124.84(10) . 2_565 ?
P2 O2 Mn1 128.71(10) . . ?
P1 O3 Mn1 154.85(12) . . ?


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
N2 HB O1 0.89 2.05 2.8461(18) 147.7 7_565 yes
N2 HB O3 0.89 2.48 3.122(3) 129.6 8_656 yes
N2 HC O1 0.89 2.05 2.8461(18) 147.7 . yes
N2 HC O3 0.89 2.48 3.122(3) 129.6 2_565 yes
N1 HA O2 0.86 2.20 2.977(2) 150.9 7_565 yes

_refine_diff_density_max         0.435
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.080

_shelx_res_file                  
;
TITL mhyd_mn_po2_30m_a.res in Pnma
    100K.res
    created by SHELXL-2018/3 at 13:43:56 on 02-Mar-2020
REM Old TITL MHyd_Mn_PO2_30m in Pnma
REM SHELXT solution in Pnma
REM R1 0.121, Rweak 0.143, Alpha 0.033, Orientation as input

CELL 0.71073   9.2009 13.2604 8.5408   90 90 90
ZERR 4 0.000586 0.00076 0.000608 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,-Z
SYMM 0.5+X,0.5-Y,0.5-Z
SFAC H N O P Mn C
UNIT 52 8 24 12 4 4
L.S. 10 0 0
PLAN  20
BOND $H
list 4
fmap 2 53
shel 10 0.82
omit 0 4 0
ACTA
bond $H
htab
EQIV $6 x, -y+1/2, z
HTAB N2 O1_$6
EQIV $7 -x+1/2, y-1/2, z+1/2
HTAB N2 O3_$7
HTAB N2 O1
EQIV $1 -x+1/2, -y+1, z+1/2
HTAB N2 O3_$1
HTAB N1 O2_$6

WGHT    0.036900    1.707500
EXTI    0.002275
FVAR       0.35192
MN1   5    0.500000    0.500000    0.500000    10.50000    0.00667    0.00479 =
         0.02322   -0.00010   -0.00041   -0.00014
P1    4    0.489997    0.750000    0.650497    10.50000    0.01147    0.00731 =
         0.02533    0.00000   -0.00119    0.00000
AFIX  23
H1A   1    0.591560    0.750001    0.680953    10.50000   -1.20000
H1B   1    0.432834    0.750000    0.745925    10.50000   -1.20000
AFIX   0
P2    4    0.173766    0.516450    0.664897    11.00000    0.01515    0.00800 =
         0.02901    0.00075    0.00557    0.00020
AFIX  23
H2A   1    0.113083    0.557074    0.596729    11.00000   -1.20000
H2B   1    0.228395    0.562375    0.730860    11.00000   -1.20000
AFIX   0
O1    3    0.076192    0.454384    0.768161    11.00000    0.01330    0.01103 =
         0.02651   -0.00085    0.00411   -0.00166
O2    3    0.279331    0.459284    0.565019    11.00000    0.01073    0.01269 =
         0.02867   -0.00221    0.00343   -0.00360
O3    3    0.459987    0.654466    0.565409    11.00000    0.02104    0.00794 =
         0.03740   -0.00312   -0.00287    0.00171
N2    2    0.170490    0.250000    0.762288    10.50000    0.00811    0.00892 =
         0.02853    0.00000    0.00135    0.00000
AFIX  23
HB    1    0.123156    0.195890    0.796942    10.50000   -1.20000
HC    1    0.123156    0.304110    0.796942    10.50000   -1.20000
AFIX   0
N1    2    0.165082    0.250000    0.593361    10.50000    0.01888    0.00893 =
         0.02650    0.00000    0.00187    0.00000
AFIX   7
HA    1    0.212481    0.199570    0.555645    11.00000   -1.20000
AFIX   0
C1    6    0.318744    0.250000    0.831987    10.50000    0.00919    0.01447 =
         0.03239    0.00000   -0.00138    0.00000
AFIX 133
HD    1    0.370645    0.191246    0.797540    10.50000   -1.50000
HE    1    0.311276    0.249292    0.944095    10.50000   -1.50000
HF    1    0.369938    0.309462    0.799284    10.50000   -1.50000

AFIX   0
HKLF 4




REM  mhyd_mn_po2_30m_a.res in Pnma
REM wR2 = 0.0829, GooF = S = 1.183, Restrained GooF = 1.183 for all data
REM R1 = 0.0284 for 1014 Fo > 4sig(Fo) and 0.0290 for all 1037 data
REM 69 parameters refined using 0 restraints

END

WGHT      0.0365      1.7088

REM Instructions for potential hydrogen bonds
HTAB N2 O1_$6
HTAB N2 O3_$7
HTAB N2 O1
HTAB N2 O3_$1
HTAB N1 O2_$6

REM Highest difference peak  0.435,  deepest hole -0.466,  1-sigma level  0.080
Q1    1   0.4057  0.7500  0.8204  10.50000  0.05    0.43
Q2    1   0.6520  0.7500  0.7221  10.50000  0.05    0.43
Q3    1   0.2582  0.5947  0.7641  11.00000  0.05    0.41
Q4    1   0.0793  0.5799  0.5435  11.00000  0.05    0.40
Q5    1   0.4826  0.6996  0.5716  11.00000  0.05    0.32
Q6    1   0.1144  0.4788  0.7260  11.00000  0.05    0.29
Q7    1   0.1405  0.4606  0.7418  11.00000  0.05    0.29
Q8    1   0.2397  0.2500  0.7972  10.50000  0.05    0.26
Q9    1   0.0887  0.4354  0.8037  11.00000  0.05    0.25
Q10   1   0.2769  0.4829  0.5067  11.00000  0.05    0.23
Q11   1   0.5059  0.4521  0.4233  11.00000  0.05    0.22
Q12   1   0.0663  0.4165  0.7184  11.00000  0.05    0.22
Q13   1   0.4596  0.6581  0.4996  11.00000  0.05    0.22
Q14   1   0.2398  0.5048  0.5647  11.00000  0.05    0.22
Q15   1   0.2064  0.4787  0.5854  11.00000  0.05    0.21
Q16   1   0.5059  0.4525  0.5815  11.00000  0.05    0.21
Q17   1   0.2458  0.4210  0.5429  11.00000  0.05    0.18
Q18   1   0.0739  0.2500  0.5433  10.50000  0.05    0.18
Q19   1   0.0209  0.4766  0.7847  11.00000  0.05    0.18
Q20   1   0.5859  0.7500  0.8332  10.50000  0.05    0.16
;
_shelx_res_checksum              68266
####################################################################### 
# 
# 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_rt
_database_code_depnum_ccdc_archive 'CCDC 1989065'
loop_
_audit_author_name
_audit_author_address
'Anna Gagor'
;ILT SR PAS Wroclaw Poland
Poland
;
_audit_update_record             
;
2020-03-09 deposited with the CCDC.	2020-05-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C H13 Mn N2 O6 P3'
_chemical_formula_weight         296.98

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

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

_cell_length_a                   9.4005(6)
_cell_length_b                   13.2990(8)
_cell_length_c                   8.6191(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1077.54(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    1413
_cell_measurement_theta_min      2.7890
_cell_measurement_theta_max      29.0770

_exptl_crystal_description       prism
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.831
_exptl_crystal_F_000             608
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.09
_exptl_absorpt_coefficient_mu    1.672
_diffrn_ambient_temperature      295(2)
_exptl_absorpt_correction_T_min  0.83777
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.869
_oxdiff_exptl_absorpt_empirical_full_max 1.265
_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_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_detector_area_resol_mean 10.6249
_diffrn_reflns_number            3038
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_av_R_equivalents  0.0223
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_theta_min         2.816
_diffrn_reflns_theta_max         25.669
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1067
_reflns_number_gt                873
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0520P)²+1.2782P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.0162(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1067
_refine_ls_number_parameters     69
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0343
_refine_ls_wR_factor_ref         0.1002
_refine_ls_wR_factor_gt          0.0929
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.054
_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
Mn1 Mn 0.500000 0.500000 0.500000 0.0211(3) Uani 1 2 d S . P . .
P1 P 0.49002(13) 0.750000 0.64708(14) 0.0302(3) Uani 1 2 d S T P . .
H1A H 0.588373 0.749999 0.681104 0.036 Uiso 1 2 calc R U P . .
H1B H 0.431209 0.750000 0.739553 0.036 Uiso 1 2 calc R U P . .
P2 P 0.18166(11) 0.51629(7) 0.67096(12) 0.0404(3) Uani 1 1 d . . . . .
H2A H 0.122681 0.555166 0.600751 0.048 Uiso 1 1 calc R U . . .
H2B H 0.233171 0.563682 0.735488 0.048 Uiso 1 1 calc R U . . .
O1 O 0.0859(2) 0.45618(16) 0.7735(3) 0.0354(6) Uani 1 1 d . . . . .
O2 O 0.2869(2) 0.45982(17) 0.5768(3) 0.0379(6) Uani 1 1 d . . . . .
O3 O 0.4640(3) 0.65523(18) 0.5639(3) 0.0475(7) Uani 1 1 d . . . . .
N2 N 0.1772(4) 0.250000 0.7627(5) 0.0304(8) Uani 1 2 d S T P . .
HB H 0.130826 0.196081 0.797165 0.036 Uiso 0.5 1 calc R U P . .
HC H 0.130826 0.303919 0.797165 0.036 Uiso 0.5 1 calc R U P . .
N1 N 0.1707(5) 0.250000 0.5956(4) 0.0383(10) Uani 1 2 d S T P . .
HA H 0.222836 0.201908 0.558817 0.046 Uiso 1 1 d R U . . .
C1 C 0.3201(5) 0.250000 0.8319(6) 0.0418(12) Uani 1 2 d S T P . .
HD H 0.371350 0.191662 0.797459 0.063 Uiso 0.5 1 calc R U P . .
HE H 0.312246 0.248816 0.942887 0.063 Uiso 0.5 2 calc R U P . .
HF H 0.370174 0.309523 0.800353 0.063 Uiso 0.5 1 calc R U P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mn1 0.0223(4) 0.0157(4) 0.0253(4) 0.0000(2) -0.0009(2) -0.0006(2)
P1 0.0429(7) 0.0185(6) 0.0293(6) 0.000 -0.0045(5) 0.000
P2 0.0502(6) 0.0249(5) 0.0460(6) 0.0037(4) 0.0222(5) 0.0023(4)
O1 0.0431(13) 0.0301(11) 0.0331(12) -0.0036(10) 0.0158(11) -0.0053(10)
O2 0.0325(12) 0.0335(12) 0.0476(14) -0.0052(12) 0.0139(11) -0.0080(10)
O3 0.0608(16) 0.0218(11) 0.0599(17) -0.0100(11) -0.0026(14) 0.0021(12)
N2 0.0271(19) 0.0250(17) 0.039(2) 0.000 0.0053(17) 0.000
N1 0.050(3) 0.031(2) 0.033(2) 0.000 0.0044(19) 0.000
C1 0.034(3) 0.047(3) 0.045(3) 0.000 0.000(2) 0.000

_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
Mn1 O3 2.163(2) 5_666 ?
Mn1 O3 2.163(2) . ?
Mn1 O2 2.176(2) 5_666 ?
Mn1 O2 2.176(2) . ?
Mn1 O1 2.192(2) 6_657 ?
Mn1 O1 2.192(2) 2_564 ?
P1 O3 1.470(2) . ?
P1 O3 1.470(2) 7_575 ?
P1 H1A 0.9700 . ?
P1 H1B 0.9700 . ?
P2 O2 1.484(2) . ?
P2 O1 1.493(2) . ?
P2 H2A 0.9700 . ?
P2 H2B 0.9700 . ?
N2 N1 1.442(5) . ?
N2 C1 1.470(6) . ?
N2 HB 0.8900 . ?
N2 HC 0.8900 . ?
N1 HA 0.8657 . ?
C1 HD 0.9600 . ?
C1 HE 0.9600 . ?
C1 HF 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Mn1 O3 180.00(15) 5_666 . ?
O3 Mn1 O2 90.74(9) 5_666 5_666 ?
O3 Mn1 O2 89.26(10) . 5_666 ?
O3 Mn1 O2 89.26(10) 5_666 . ?
O3 Mn1 O2 90.74(10) . . ?
O2 Mn1 O2 180.0 5_666 . ?
O3 Mn1 O1 85.16(10) 5_666 6_657 ?
O3 Mn1 O1 94.84(10) . 6_657 ?
O2 Mn1 O1 89.84(9) 5_666 6_657 ?
O2 Mn1 O1 90.16(9) . 6_657 ?
O3 Mn1 O1 94.84(10) 5_666 2_564 ?
O3 Mn1 O1 85.16(10) . 2_564 ?
O2 Mn1 O1 90.16(9) 5_666 2_564 ?
O2 Mn1 O1 89.84(9) . 2_564 ?
O1 Mn1 O1 180.0 6_657 2_564 ?
O3 P1 O3 118.0(2) . 7_575 ?
O3 P1 H1A 107.8 . . ?
O3 P1 H1A 107.8 7_575 . ?
O3 P1 H1B 107.8 . . ?
O3 P1 H1B 107.8 7_575 . ?
H1A P1 H1B 107.1 . . ?
O2 P2 O1 117.05(13) . . ?
O2 P2 H2A 108.0 . . ?
O1 P2 H2A 108.0 . . ?
O2 P2 H2B 108.0 . . ?
O1 P2 H2B 108.0 . . ?
H2A P2 H2B 107.3 . . ?
P2 O1 Mn1 127.35(13) . 2_565 ?
P2 O2 Mn1 130.98(14) . . ?
P1 O3 Mn1 156.37(18) . . ?
N1 N2 C1 116.3(4) . . ?
N1 N2 HB 108.2 . . ?
C1 N2 HB 108.2 . . ?
N1 N2 HC 108.2 . . ?
C1 N2 HC 108.2 . . ?
HB N2 HC 107.4 . . ?
N2 N1 HA 110.0 . . ?
N2 N1 HA 110.0(8) . 7_565 ?
HA N1 HA 95.2 . 7_565 ?
N2 C1 HD 109.5 . . ?
N2 C1 HE 109.5 . . ?
HD C1 HE 109.5 . . ?
N2 C1 HF 109.5 . . ?
HD C1 HF 109.5 . . ?
HE C1 HF 109.5 . . ?

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
N2 HB O1 0.89 2.08 2.875(2) 148.4 7_565 yes
N2 HB O3 0.89 2.53 3.176(5) 130.5 8_656 yes
N2 HC O1 0.89 2.08 2.875(2) 148.4 . yes
N2 HC O3 0.89 2.53 3.176(5) 130.5 2_565 yes
N1 HA O2 0.87 2.24 3.001(3) 146.8 7_565 yes

_refine_diff_density_max         0.364
_refine_diff_density_min         -0.564
_refine_diff_density_rms         0.084

_shelx_res_file                  
;
TITL mhyd_mn_po2_30m_a.res in Pnma
    rt.res
    created by SHELXL-2018/3 at 15:10:16 on 05-Feb-2020
REM Old TITL MHyd_Mn_PO2_30m in Pnma
REM SHELXT solution in Pnma
REM R1 0.121, Rweak 0.143, Alpha 0.033, Orientation as input

CELL 0.71073  9.400544 13.298978 8.619116   90 90 90
ZERR 4 0.000586 0.00076 0.000608 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,-Z
SYMM 0.5+X,0.5-Y,0.5-Z
SFAC H N O P Mn C
UNIT 52 8 24 12 4 4
L.S. 10 0 0
PLAN  20
BOND $H
list 4
fmap 2 53
shel 10 0.82
omit 0 4 0
ACTA
bond $H
htab
EQIV $6 x, -y+1/2, z
HTAB N2  O1_$6
EQIV $7 -x+1/2, y-1/2, z+1/2
HTAB N2  O3_$7
HTAB N2  O1
EQIV $1 -x+1/2, -y+1, z+1/2
HTAB N2  O3_$1
HTAB N1   O2_$6

WGHT    0.052000    1.278200
EXTI    0.016166
FVAR       5.72383
Mn1   5    0.500000    0.500000    0.500000    10.50000    0.02231    0.01569 =
         0.02528   -0.00003   -0.00085   -0.00062
P1    4    0.490017    0.750000    0.647079    10.50000    0.04292    0.01851 =
         0.02929    0.00000   -0.00446    0.00000
AFIX  23
H1A   1    0.588373    0.749999    0.681104    10.50000   -1.20000
H1B   1    0.431209    0.750000    0.739553    10.50000   -1.20000
AFIX   0
P2    4    0.181665    0.516295    0.670963    11.00000    0.05017    0.02494 =
         0.04603    0.00373    0.02224    0.00233
AFIX  23
H2A   1    0.122681    0.555166    0.600751    11.00000   -1.20000
H2B   1    0.233171    0.563682    0.735488    11.00000   -1.20000
AFIX   0
O1    3    0.085871    0.456184    0.773451    11.00000    0.04307    0.03012 =
         0.03310   -0.00355    0.01578   -0.00526
O2    3    0.286923    0.459821    0.576784    11.00000    0.03254    0.03350 =
         0.04758   -0.00524    0.01393   -0.00801
O3    3    0.464015    0.655227    0.563916    11.00000    0.06081    0.02184 =
         0.05988   -0.01000   -0.00262    0.00213
N2    2    0.177179    0.250000    0.762742    10.50000    0.02708    0.02501 =
         0.03901    0.00000    0.00530    0.00000
AFIX  23
HB    1    0.130826    0.196081    0.797165    10.50000   -1.20000
HC    1    0.130826    0.303919    0.797165    10.50000   -1.20000
AFIX   0
N1    2    0.170735    0.250000    0.595611    10.50000    0.04988    0.03146 =
         0.03348    0.00000    0.00440    0.00000
AFIX   7
HA    1    0.222836    0.201908    0.558817    11.00000   -1.20000
AFIX   0
C1    6    0.320137    0.250000    0.831855    10.50000    0.03362    0.04657 =
         0.04527    0.00000    0.00001    0.00000
AFIX 133
HD    1    0.371350    0.191662    0.797459    10.50000   -1.50000
HE    1    0.312246    0.248816    0.942887    10.50000   -1.50000
HF    1    0.370174    0.309523    0.800353    10.50000   -1.50000

AFIX   0
HKLF 4




REM  mhyd_mn_po2_30m_a.res in Pnma
REM wR2 = 0.1002, GooF = S = 1.054, Restrained GooF = 1.054 for all data
REM R1 = 0.0343 for 873 Fo > 4sig(Fo) and 0.0432 for all 1067 data
REM 69 parameters refined using 0 restraints

END

WGHT      0.0501      1.3529

REM Instructions for potential hydrogen bonds
HTAB N2  O1_$6
HTAB N2  O3_$7
HTAB N2  O1
HTAB N2  O3_$1
HTAB N1   O2_$6

REM Highest difference peak  0.364,  deepest hole -0.564,  1-sigma level  0.084
Q1    1   0.6539  0.7500  0.7207  10.50000  0.05    0.36
Q2    1   0.0015  0.2500  0.8529  10.50000  0.05    0.33
Q3    1   0.4730  0.6641  0.5152  11.00000  0.05    0.30
Q4    1   0.3924  0.7500  0.8231  10.50000  0.05    0.28
Q5    1   0.5409  0.6542  0.5978  11.00000  0.05    0.28
Q6    1   0.3359  0.7625  0.7488  11.00000  0.05    0.27
Q7    1   0.3498  0.2500  0.7562  10.50000  0.05    0.25
Q8    1   0.4412  0.6797  0.6201  11.00000  0.05    0.24
Q9    1   0.2509  0.5805  0.7915  11.00000  0.05    0.23
Q10   1   0.4636  0.6606  0.6410  11.00000  0.05    0.23
Q11   1   0.1794  0.6177  0.6969  11.00000  0.05    0.20
Q12   1   0.0621  0.5006  0.7787  11.00000  0.05    0.20
Q13   1   0.0934  0.2500  0.9527  10.50000  0.05    0.20
Q14   1   0.1507  0.4416  0.7207  11.00000  0.05    0.19
Q15   1   0.5338  0.6099  0.5245  11.00000  0.05    0.19
Q16   1   0.2832  0.5202  0.5721  11.00000  0.05    0.19
Q17   1   0.1513  0.4829  0.6006  11.00000  0.05    0.19
Q18   1   0.0598  0.5552  0.5577  11.00000  0.05    0.19
Q19   1   0.1342  0.4360  0.8458  11.00000  0.05    0.18
Q20   1   0.5221  0.7202  0.4532  11.00000  0.05    0.18
;
_shelx_res_checksum              47212
