 
data_shelx
 
_audit_creation_method            'SHELXL-2014/7'
_shelx_SHELXL_version_number      '2014/7'
_chemical_name_systematic         'dinickel diphosphate dihydrate'
_chemical_name_common             'nickel diphosphate hydrate'
_chemical_melting_point           ?
_chemical_formula_moiety          'Ni2 P2 O7,(H2O)2'
_chemical_formula_sum
 'H4 Ni2 O9 P2' 
_chemical_formula_weight          327.39

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'
 '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'
 'Ni'  'Ni'   0.3393   1.1124
 '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                    6.25170(10)
_cell_length_b                    13.7892(3)
_cell_length_c                    7.2894(2)
_cell_angle_alpha                 90
_cell_angle_beta                  94.507(2)
_cell_angle_gamma                 90
_cell_volume                      626.45(2)
_cell_formula_units_Z             4
_cell_measurement_temperature     164(2)
_cell_measurement_reflns_used     4732
_cell_measurement_theta_min       3.1610
_cell_measurement_theta_max       32.3990
 
_exptl_crystal_description        'flattened'
_exptl_crystal_colour             'pale green'
_exptl_crystal_density_meas       'not measured'
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     3.471          
_exptl_crystal_F_000              648
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.100
_exptl_crystal_size_mid           0.080
_exptl_crystal_size_min           0.029
_exptl_absorpt_coefficient_mu     6.548
_shelx_estimated_absorpt_T_min    0.560
_shelx_estimated_absorpt_T_max    0.833
_exptl_absorpt_correction_type    'analytical'
_exptl_absorpt_correction_T_min   0.886
_exptl_absorpt_correction_T_max   0.957
_exptl_absorpt_process_details    
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       164(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type   'Xcalibur, AtlasS2, Gemini'
_diffrn_measurement_method        'ω scans'
_diffrn_detector_area_resol_mean  5.2283
_diffrn_reflns_number             6852
_diffrn_reflns_av_unetI/netI      0.0185
_diffrn_reflns_av_R_equivalents   0.0177
_diffrn_reflns_limit_h_min        -8
_diffrn_reflns_limit_h_max        8
_diffrn_reflns_limit_k_min        -19
_diffrn_reflns_limit_k_max        19
_diffrn_reflns_limit_l_min        -10
_diffrn_reflns_limit_l_max        10
_diffrn_reflns_theta_min          2.954
_diffrn_reflns_theta_max          29.991
_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              1822
_reflns_number_gt                 1700
_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 1.171.40.67a (Rigaku OD, 2019)'
_computing_cell_refinement        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction         'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_structure_solution     'SHELXS (Sheldrick, 2015)'
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics     'DIAMOND (Brandenburg, 2006)'
_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)+(0.0157P)²+0.3800P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    difmap
_refine_ls_hydrogen_treatment     refall
_refine_ls_extinction_method      'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef        0.0016(3)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          1822
_refine_ls_number_parameters      135
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0191
_refine_ls_R_factor_gt            0.0160
_refine_ls_wR_factor_ref          0.0389
_refine_ls_wR_factor_gt           0.0383
_refine_ls_goodness_of_fit_ref    1.125
_refine_ls_restrained_S_all       1.125
_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
Ni1 Ni 0.26753(3) 0.11435(2) 0.58497(3) 0.00381(6) Uani 1 1 d . . . . .
Ni2 Ni 0.04756(3) 0.24996(2) 0.85186(3) 0.00391(6) Uani 1 1 d . . . . .
P2 P 0.26032(7) 0.41674(3) 0.14949(6) 0.00345(9) Uani 1 1 d . . . . .
P1 P 0.06421(7) 0.31199(3) 0.43021(6) 0.00348(9) Uani 1 1 d . . . . .
O1 O 0.16688(18) 0.40781(8) 0.34815(15) 0.0044(2) Uani 1 1 d . . . . .
O2 O -0.14062(18) 0.29078(9) 0.30787(16) 0.0053(2) Uani 1 1 d . . . . .
O3 O 0.22883(18) 0.23073(9) 0.40779(16) 0.0055(2) Uani 1 1 d . . . . .
O4 O 0.19582(18) 0.02255(8) 0.37492(16) 0.0057(2) Uani 1 1 d . . . . .
O5 O 0.08545(18) 0.37282(8) 0.01641(16) 0.0051(2) Uani 1 1 d . . . . .
O6 O 0.02929(19) 0.33884(8) 0.62560(15) 0.0057(2) Uani 1 1 d . . . . .
O7 O 0.46539(18) 0.35650(9) 0.16058(16) 0.0052(2) Uani 1 1 d . . . . .
O8 O 0.2576(2) 0.00567(9) 0.77691(17) 0.0084(2) Uani 1 1 d . . . . .
O9 O 0.0632(2) 0.14883(10) 1.06083(18) 0.0090(2) Uani 1 1 d . . . . .
H1 H 0.343(5) -0.040(2) 0.802(4) 0.037(8) Uiso 1 1 d . . . . .
H2 H 0.137(5) -0.020(2) 0.772(4) 0.048(9) Uiso 1 1 d . . . . .
H3 H 0.084(6) 0.170(3) 1.166(5) 0.070(12) Uiso 1 1 d . . . . .
H4 H 0.160(7) 0.111(3) 1.039(6) 0.094(16) 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
Ni1 O4 2.0099(12) . ?
Ni1 O7 2.0486(12) 4_566 ?
Ni1 O8 2.0545(13) . ?
Ni1 O3 2.0623(12) . ?
Ni1 O5 2.0947(12) 4_666 ?
Ni1 O2 2.1294(12) 4_666 ?
Ni2 O6 2.0508(11) . ?
Ni2 O7 2.0616(12) 4_566 ?
Ni2 O9 2.0619(13) . ?
Ni2 O2 2.0777(12) 4_666 ?
Ni2 O5 2.0785(12) 1_556 ?
Ni2 O3 2.0821(12) 4_566 ?
P2 O4 1.4978(12) 2 ?
P2 O7 1.5245(12) . ?
P2 O5 1.5285(12) . ?
P2 O1 1.6083(12) . ?
P1 O6 1.5040(12) . ?
P1 O2 1.5301(12) . ?
P1 O3 1.5388(12) . ?
P1 O1 1.6048(12) . ?
O2 Ni2 2.0777(11) 4_565 ?
O2 Ni1 2.1294(12) 4_565 ?
O3 Ni2 2.0821(12) 4_665 ?
O4 P2 1.4977(12) 2_545 ?
O5 Ni2 2.0785(11) 1_554 ?
O5 Ni1 2.0947(12) 4_565 ?
O7 Ni1 2.0486(12) 4_665 ?
O7 Ni2 2.0616(12) 4_665 ?
O8 H1 0.84(3) . ?
O8 H2 0.83(3) . ?
O9 H3 0.82(4) . ?
O9 H4 0.82(4) . ?
 
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
O4 Ni1 O7 99.98(5) . 4_566 ?
O4 Ni1 O8 92.44(5) . . ?
O7 Ni1 O8 83.23(5) 4_566 . ?
O4 Ni1 O3 90.28(5) . . ?
O7 Ni1 O3 87.16(5) 4_566 . ?
O8 Ni1 O3 170.33(5) . . ?
O4 Ni1 O5 91.75(5) . 4_666 ?
O7 Ni1 O5 163.71(5) 4_566 4_666 ?
O8 Ni1 O5 107.71(5) . 4_666 ?
O3 Ni1 O5 81.47(4) . 4_666 ?
O4 Ni1 O2 177.19(5) . 4_666 ?
O7 Ni1 O2 82.72(4) 4_566 4_666 ?
O8 Ni1 O2 87.09(5) . 4_666 ?
O3 Ni1 O2 90.64(5) . 4_666 ?
O5 Ni1 O2 85.76(4) 4_666 4_666 ?
O6 Ni2 O7 83.48(5) . 4_566 ?
O6 Ni2 O9 174.14(5) . . ?
O7 Ni2 O9 90.74(5) 4_566 . ?
O6 Ni2 O2 91.78(5) . 4_666 ?
O7 Ni2 O2 83.69(5) 4_566 4_666 ?
O9 Ni2 O2 86.59(5) . 4_666 ?
O6 Ni2 O5 88.49(5) . 1_556 ?
O7 Ni2 O5 169.02(5) 4_566 1_556 ?
O9 Ni2 O5 97.37(5) . 1_556 ?
O2 Ni2 O5 104.10(5) 4_666 1_556 ?
O6 Ni2 O3 95.01(5) . 4_566 ?
O7 Ni2 O3 91.84(5) 4_566 4_566 ?
O9 Ni2 O3 86.12(5) . 4_566 ?
O2 Ni2 O3 171.40(5) 4_666 4_566 ?
O5 Ni2 O3 81.38(5) 1_556 4_566 ?
O4 P2 O7 112.09(7) 2 . ?
O4 P2 O5 116.05(7) 2 . ?
O7 P2 O5 111.98(7) . . ?
O4 P2 O1 105.34(7) 2 . ?
O7 P2 O1 105.90(6) . . ?
O5 P2 O1 104.41(6) . . ?
O6 P1 O2 114.95(7) . . ?
O6 P1 O3 115.33(7) . . ?
O2 P1 O3 109.57(7) . . ?
O6 P1 O1 104.03(6) . . ?
O2 P1 O1 106.33(6) . . ?
O3 P1 O1 105.63(6) . . ?
P1 O1 P2 125.65(7) . . ?
P1 O2 Ni2 135.58(7) . 4_565 ?
P1 O2 Ni1 119.37(7) . 4_565 ?
Ni2 O2 Ni1 94.81(5) 4_565 4_565 ?
P1 O3 Ni1 123.14(7) . . ?
P1 O3 Ni2 125.87(7) . 4_665 ?
Ni1 O3 Ni2 98.93(5) . 4_665 ?
P2 O4 Ni1 132.22(7) 2_545 . ?
P2 O5 Ni2 137.11(7) . 1_554 ?
P2 O5 Ni1 117.38(7) . 4_565 ?
Ni2 O5 Ni1 98.01(5) 1_554 4_565 ?
P1 O6 Ni2 127.69(7) . . ?
P2 O7 Ni1 131.92(7) . 4_665 ?
P2 O7 Ni2 125.99(7) . 4_665 ?
Ni1 O7 Ni2 97.80(5) 4_665 4_665 ?
Ni1 O8 H1 130.2(19) . . ?
Ni1 O8 H2 111(2) . . ?
H1 O8 H2 104(3) . . ?
Ni2 O9 H3 117(3) . . ?
Ni2 O9 H4 106(3) . . ?
H3 O9 H4 110(3) . . ?
 
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 
O8 H1 O6  0.84(3) 1.90(3) 2.7245(17) 165(3) 2_546
O8 H2 O4  0.83(3) 2.27(3) 2.9863(17) 145(3) 3_556
O9 H3 O3  0.82(4) 2.09(4) 2.8866(18) 163(3) 1_556
O9 H4 O6  0.82(4) 2.44(4) 2.9200(18) 118(3) 4_666
 
_refine_diff_density_max    0.559
_refine_diff_density_min   -0.394
_refine_diff_density_rms    0.091

# start Validation Reply Form
_vrf_PLAT430_shelx
;
PROBLEM: Short Inter D...A Contact  O2       ..O7       .       2.76 Ang.  
RESPONSE: This short contact  O2..O7 of 2.76 Ang is the edge of Ni-octahedron
;
_vrf_PLAT906_shelx
;
PROBLEM: Large K Value in the Analysis of Variance ......      2.872 Check 
RESPONSE: The K value is large exclusively for weak reflections with
Fc/Fcmax lower than 0.022
;
# end Validation Reply Form



