# Electronic Supplementary Material (ESI) for CrystEngComm.
# 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_x
_database_code_depnum_ccdc_archive 'CCDC 2056695'
loop_
_audit_author_name
_audit_author_address
'xing huang'
;Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences
China
;
_audit_update_record             
;
2021-01-17 deposited with the CCDC.	2021-03-11 downloaded from the CCDC.
;
_audit_creation_date             2020-10-22
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        CaNi2(SeO3)3(1.5H2O)
_chemical_formula_moiety         '0.5(Ca2 H6 Ni4 O21 Se6)'
_chemical_formula_sum            'Ca H3 Ni2 O10.50 Se3'
_chemical_formula_weight         565.40
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ca Ca 0.2262 0.3064 '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'
Ni Ni 0.3393 1.1124 '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'
Se Se -0.0929 2.2259 '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           11
_space_group_name_H-M_alt        'P 1 21/m 1'
_space_group_name_Hall           '-P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'

_cell_length_a                   7.7605(2)
_cell_length_b                   7.33360(10)
_cell_length_c                   8.9393(2)
_cell_angle_alpha                90
_cell_angle_beta                 115.115(3)
_cell_angle_gamma                90
_cell_volume                     460.66(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4342
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      33.0470
_cell_measurement_theta_min      2.5290
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    16.543
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.09842
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46c (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    4.076
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             530
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0206
_diffrn_reflns_av_unetI/netI     0.0210
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.943
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4696
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.118
_diffrn_reflns_theta_min         2.516
_diffrn_ambient_temperature      298
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -118.00  62.00   0.50    4.00    --  -28.00  45.00 180.00  360
  2  ω   -118.00  22.00   0.50    4.00    --  -28.00  45.00  90.00  280
  3  ω   -118.00 -43.50   0.50    4.00    --  -28.00  45.00   0.00  149
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0744116000
_diffrn_orient_matrix_UB_12      0.0580903000
_diffrn_orient_matrix_UB_13      0.0028347000
_diffrn_orient_matrix_UB_21      -0.0471255000
_diffrn_orient_matrix_UB_22      0.0758325000
_diffrn_orient_matrix_UB_23      0.0150444000
_diffrn_orient_matrix_UB_31      0.0493200000
_diffrn_orient_matrix_UB_32      -0.0151681000
_diffrn_orient_matrix_UB_33      0.0862915000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1673
_reflns_number_total             1766
_reflns_odcompleteness_completeness 94.25
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     33.04
_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       'CrysAlisPro 1.171.39.46c (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46c (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46c (Rigaku OD, 2018)'
_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         1.616
_refine_diff_density_min         -1.110
_refine_diff_density_rms         0.218
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         1766
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0267
_refine_ls_R_factor_gt           0.0250
_refine_ls_restrained_S_all      1.097
_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)+(0.0349P)²+1.2867P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0645
_refine_ls_wR_factor_ref         0.0652
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 H1WA-H1WA_$1
 2.2 with sigma of 0.01
 O1W-H1WA = O1W-H1WB
 0.82 with sigma of 0.01
 H1WA-H1WB
 1.39 with sigma of 0.01
 H1WA-Ca1 \\sim H1WB-Ca1
 with sigma of 0.02
 H1BA-O1B \\sim H1BB-O1B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O1W \\sim O1B: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
4. Others
 Fixed Sof: O1W(0.5) H1WA(0.5) H1WB(0.5) O1B(0.25) H1BA(0.25) H1BB(0.25)
5.a Riding coordinates:
 O1B(H1BA,H1BB)
;
_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
Ni1 Ni 0.17566(5) 0.55836(4) 0.31368(4) 0.00793(8) Uani 1 1 d . . . . .
Se1 Se 0.00571(5) 0.250000 0.04630(4) 0.00805(8) Uani 1 2 d S T P . .
Se2 Se 0.03168(5) 0.250000 0.48116(4) 0.00757(8) Uani 1 2 d S T P A .
Se3 Se 0.53616(5) 0.250000 0.32552(4) 0.00748(8) Uani 1 2 d S T P . .
O1 O -0.0462(3) 0.4269(3) 0.1415(2) 0.0126(4) Uani 1 1 d . . . . .
O2 O -0.1920(4) 0.250000 -0.1431(3) 0.0091(5) Uani 1 2 d S T P . .
O3 O 0.1934(3) 0.4230(3) 0.5192(2) 0.0106(3) Uani 1 1 d . . . . .
O4 O 0.0144(4) 0.250000 0.6658(3) 0.0101(5) Uani 1 2 d S T P . .
O5 O 0.3935(3) 0.4343(3) 0.2743(3) 0.0128(4) Uani 1 1 d . . . . .
O6 O 0.6194(4) 0.250000 0.5379(3) 0.0109(5) Uani 1 2 d S T P A .
Ca1 Ca 0.46928(11) 0.250000 0.71527(11) 0.01446(15) Uani 1 2 d DS T P . .
O1W O 0.406(2) 0.415(3) 0.9263(15) 0.125(7) Uani 0.5 1 d D U . A 1
H1WA H 0.441(7) 0.370(5) 1.019(3) 0.187 Uiso 0.5 1 d DR . . B 1
H1WB H 0.31(2) 0.48(3) 0.897(6) 0.187 Uiso 0.5 1 d DR . . C 1
O1B O 0.3676(18) 0.250000 0.9217(16) 0.097(8) Uani 0.5 2 d DS TU P A 2
H1BA H 0.253935 0.250000 0.869843 0.146 Uiso 0.5 2 d DRS T P A 2
H1BB H 0.405345 0.230130 1.019863 0.146 Uiso 0.25 1 d DR . . 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
Ni1 O1 2.003(2) . ?
Ni1 O2 2.116(2) 3_565 ?
Ni1 O3 2.0407(19) . ?
Ni1 O4 2.101(2) 3_566 ?
Ni1 O5 2.077(2) . ?
Ni1 O6 2.115(2) 3_666 ?
Se1 O1 1.691(2) 4_565 ?
Se1 O1 1.691(2) . ?
Se1 O2 1.737(3) . ?
Se2 O3 1.7142(19) . ?
Se2 O3 1.7142(19) 4_565 ?
Se2 O4 1.712(3) . ?
Se2 Ca1 3.1432(9) . ?
Se3 O5 1.6829(19) . ?
Se3 O5 1.6830(19) 4_565 ?
Se3 O6 1.726(3) . ?
O2 Ca1 2.385(3) 1_454 ?
O3 Ca1 2.466(2) . ?
O5 Ca1 2.534(2) 3_666 ?
O6 Ca1 2.333(3) . ?
Ca1 O1W 2.458(13) 4_565 ?
Ca1 O1W 2.458(13) . ?
Ca1 O1B 2.294(13) . ?

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 Ni1 O2 93.48(9) . 3_565 ?
O1 Ni1 O3 99.51(8) . . ?
O1 Ni1 O4 89.02(9) . 3_566 ?
O1 Ni1 O5 98.90(8) . . ?
O1 Ni1 O6 166.89(8) . 3_666 ?
O3 Ni1 O2 165.85(8) . 3_565 ?
O3 Ni1 O4 91.61(9) . 3_566 ?
O3 Ni1 O5 101.01(8) . . ?
O3 Ni1 O6 90.74(9) . 3_666 ?
O4 Ni1 O2 82.97(9) 3_566 3_565 ?
O4 Ni1 O6 82.50(9) 3_566 3_666 ?
O5 Ni1 O2 82.35(9) . 3_565 ?
O5 Ni1 O4 163.70(8) . 3_566 ?
O5 Ni1 O6 87.03(9) . 3_666 ?
O6 Ni1 O2 75.63(9) 3_666 3_565 ?
O1 Se1 O1 100.19(15) 4_565 . ?
O1 Se1 O2 100.97(9) . . ?
O1 Se1 O2 100.97(9) 4_565 . ?
O3 Se2 O3 95.51(13) . 4_565 ?
O3 Se2 Ca1 51.31(7) 4_565 . ?
O3 Se2 Ca1 51.31(7) . . ?
O4 Se2 O3 99.16(9) . . ?
O4 Se2 O3 99.16(9) . 4_565 ?
O4 Se2 Ca1 82.11(10) . . ?
O5 Se3 O5 106.86(14) . 4_565 ?
O5 Se3 O6 101.26(9) . . ?
O5 Se3 O6 101.27(9) 4_565 . ?
Se1 O1 Ni1 116.44(11) . . ?
Ni1 O2 Ni1 83.22(10) 2_545 3_565 ?
Ni1 O2 Ca1 90.41(8) 2_545 1_454 ?
Ni1 O2 Ca1 90.41(8) 3_565 1_454 ?
Se1 O2 Ni1 113.85(11) . 2_545 ?
Se1 O2 Ni1 113.85(11) . 3_565 ?
Se1 O2 Ca1 146.72(15) . 1_454 ?
Ni1 O3 Ca1 126.62(9) . . ?
Se2 O3 Ni1 114.68(10) . . ?
Se2 O3 Ca1 95.84(8) . . ?
Ni1 O4 Ni1 83.97(10) 2_546 3_566 ?
Se2 O4 Ni1 115.44(11) . 3_566 ?
Se2 O4 Ni1 115.44(11) . 2_546 ?
Ni1 O5 Ca1 87.31(7) . 3_666 ?
Se3 O5 Ni1 142.60(12) . . ?
Se3 O5 Ca1 120.40(10) . 3_666 ?
Ni1 O6 Ni1 83.29(10) 3_666 2_646 ?
Ni1 O6 Ca1 91.89(9) 2_646 . ?
Ni1 O6 Ca1 91.89(9) 3_666 . ?
Se3 O6 Ni1 121.38(11) . 2_646 ?
Se3 O6 Ni1 121.38(11) . 3_666 ?
Se3 O6 Ca1 133.29(15) . . ?
Ni1 Ca1 Ni1 52.104(17) 3_666 2_646 ?
Se2 Ca1 Ni1 132.09(3) . 2_646 ?
Se2 Ca1 Ni1 132.09(3) . 3_666 ?
O2 Ca1 Ni1 41.41(5) 1_656 2_646 ?
O2 Ca1 Ni1 41.41(5) 1_656 3_666 ?
O2 Ca1 Se2 171.65(7) 1_656 . ?
O2 Ca1 O3 143.72(6) 1_656 4_565 ?
O2 Ca1 O3 143.72(6) 1_656 . ?
O2 Ca1 O5 68.22(5) 1_656 3_666 ?
O2 Ca1 O5 68.22(5) 1_656 2_646 ?
O2 Ca1 O1W 97.3(3) 1_656 4_565 ?
O2 Ca1 O1W 97.3(4) 1_656 . ?
O3 Ca1 Ni1 103.54(5) 4_565 2_646 ?
O3 Ca1 Ni1 103.54(5) . 3_666 ?
O3 Ca1 Ni1 133.33(6) 4_565 3_666 ?
O3 Ca1 Ni1 133.33(6) . 2_646 ?
O3 Ca1 Se2 32.86(5) 4_565 . ?
O3 Ca1 Se2 32.86(5) . . ?
O3 Ca1 O3 61.94(9) . 4_565 ?
O3 Ca1 O5 77.33(6) . 3_666 ?
O3 Ca1 O5 136.14(7) . 2_646 ?
O3 Ca1 O5 136.14(7) 4_565 3_666 ?
O3 Ca1 O5 77.32(6) 4_565 2_646 ?
O5 Ca1 Ni1 40.42(5) 2_646 2_646 ?
O5 Ca1 Ni1 92.37(5) 3_666 2_646 ?
O5 Ca1 Ni1 40.42(5) 3_666 3_666 ?
O5 Ca1 Ni1 92.37(5) 2_646 3_666 ?
O5 Ca1 Se2 110.06(5) 3_666 . ?
O5 Ca1 Se2 110.06(5) 2_646 . ?
O5 Ca1 O5 132.08(10) 3_666 2_646 ?
O6 Ca1 Ni1 41.35(5) . 3_666 ?
O6 Ca1 Ni1 41.34(5) . 2_646 ?
O6 Ca1 Se2 104.93(7) . . ?
O6 Ca1 O2 66.71(9) . 1_656 ?
O6 Ca1 O3 92.89(8) . 4_565 ?
O6 Ca1 O3 92.89(8) . . ?
O6 Ca1 O5 72.64(6) . 3_666 ?
O6 Ca1 O5 72.64(6) . 2_646 ?
O6 Ca1 O1W 147.3(4) . . ?
O6 Ca1 O1W 147.3(4) . 4_565 ?
O1W Ca1 Ni1 137.5(4) . 2_646 ?
O1W Ca1 Ni1 107.8(4) . 3_666 ?
O1W Ca1 Ni1 107.8(4) 4_565 2_646 ?
O1W Ca1 Ni1 137.5(4) 4_565 3_666 ?
O1W Ca1 Se2 90.0(3) 4_565 . ?
O1W Ca1 Se2 90.0(3) . . ?
O1W Ca1 O3 113.7(3) 4_565 . ?
O1W Ca1 O3 84.1(4) . . ?
O1W Ca1 O3 84.1(4) 4_565 4_565 ?
O1W Ca1 O3 113.7(4) . 4_565 ?
O1W Ca1 O5 129.7(5) 4_565 3_666 ?
O1W Ca1 O5 74.9(4) . 3_666 ?
O1W Ca1 O5 74.9(4) 4_565 2_646 ?
O1W Ca1 O5 129.7(5) . 2_646 ?
O1W Ca1 O1W 58.9(9) 4_565 . ?
O1B Ca1 Se2 83.8(3) . . ?
O1B Ca1 O3 94.6(3) . . ?
O1B Ca1 O6 171.3(3) . . ?
O1B Ca1 O1W 30.0(4) . 4_565 ?

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
O1W H1WA Se3 0.824(10) 2.666(19) 3.487(14) 175(6) 1_556
O1W H1WA O5 0.824(10) 2.51(5) 3.157(11) 137(6) 1_556
O1W H1WB O1 0.824(10) 2.05(8) 2.843(17) 161(21) 3_566
O1B H1BB Se3 0.81 2.48 3.277(13) 166.1 1_556
O1B H1BB O5 0.81 2.61 3.356(12) 153.5 4_566

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.927
_oxdiff_exptl_absorpt_empirical_full_min 0.570
####################################################################### 
# 
# 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_x_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2056697'
loop_
_audit_author_name
_audit_author_address
'xing huang'
;Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences
China
;
_audit_update_record             
;
2021-01-17 deposited with the CCDC.	2021-03-11 downloaded from the CCDC.
;
_audit_creation_date             2020-09-04
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        CaNi2(SeO3)3(2H2O)
_chemical_formula_moiety         '0.5(Ca2 H8 Ni4 O22 Se6)'
_chemical_formula_sum            'Ca H4 Ni2 O11 Se3'
_chemical_formula_weight         574.41
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ca Ca 0.2262 0.3064 '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'
Ni Ni 0.3393 1.1124 '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'
Se Se -0.0929 2.2259 '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           11
_space_group_name_H-M_alt        'P 1 21/m 1'
_space_group_name_Hall           '-P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'

_cell_length_a                   7.8568(4)
_cell_length_b                   7.3734(3)
_cell_length_c                   8.9697(6)
_cell_angle_alpha                90
_cell_angle_beta                 114.275(7)
_cell_angle_gamma                90
_cell_volume                     473.68(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2666
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      33.0000
_cell_measurement_theta_min      2.4730
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    16.095
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60548
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46c (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    4.027
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             540
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_av_unetI/netI     0.0499
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.943
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5495
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.046
_diffrn_reflns_theta_min         2.491
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -115.00  65.00   0.50    5.00    --  -25.00  45.00   0.00  360
  2  ω   -115.00  25.00   0.50    5.00    --  -25.00  45.00  90.00  280
  3  ω   -115.00 -35.00   0.50    5.00    --  -25.00  45.00 180.00  160
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0457118000
_diffrn_orient_matrix_UB_12      -0.0059634000
_diffrn_orient_matrix_UB_13      -0.0864412000
_diffrn_orient_matrix_UB_21      0.0836448000
_diffrn_orient_matrix_UB_22      -0.0323546000
_diffrn_orient_matrix_UB_23      -0.0027862000
_diffrn_orient_matrix_UB_31      -0.0269912000
_diffrn_orient_matrix_UB_32      -0.0903785000
_diffrn_orient_matrix_UB_33      0.0067481000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1439
_reflns_number_total             1802
_reflns_odcompleteness_completeness 94.26
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     32.97
_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       'CrysAlisPro 1.171.39.46c (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46c (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46c (Rigaku OD, 2018)'
_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         1.222
_refine_diff_density_min         -1.316
_refine_diff_density_rms         0.259
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     101
_refine_ls_number_reflns         1802
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_gt           0.0358
_refine_ls_restrained_S_all      1.031
_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)+(0.0269P)²+0.7444P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0652
_refine_ls_wR_factor_ref         0.0701
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 H1WA-H1WA_$1
 2.2 with sigma of 0.01
 O1W-H1WA = O1W-H1WB
 0.82 with sigma of 0.01
 H1WA-H1WB
 1.39 with sigma of 0.01
 H1WA-Ca1 \\sim H1WB-Ca1
 with sigma of 0.02
 H1BA-O1B \\sim H1BB-O1B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O1W \\sim O1B: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
4. Others
 Sof(O1B)=Sof(H1BA)=Sof(H1BB)=1-FVAR(1)
 Sof(O1W)=Sof(H1WA)=Sof(H1WB)=FVAR(1)
5.a Riding coordinates:
 O1B(H1BA,H1BB)
;
_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
Ni1 Ni 0.17975(7) 0.55845(7) 0.31611(6) 0.00893(12) Uani 1 1 d . . . . .
Se1 Se 0.00672(7) 0.250000 0.04154(7) 0.00857(12) Uani 1 2 d S T P . .
Se2 Se 0.03048(7) 0.250000 0.48045(7) 0.00930(12) Uani 1 2 d S T P A .
Se3 Se 0.53317(7) 0.250000 0.32773(7) 0.00841(12) Uani 1 2 d S T P . .
O1 O -0.0364(4) 0.4251(4) 0.1436(4) 0.0130(6) Uani 1 1 d . . . . .
O2 O -0.1935(5) 0.250000 -0.1401(5) 0.0091(7) Uani 1 2 d S T P . .
O3 O 0.1895(4) 0.4219(4) 0.5170(4) 0.0129(6) Uani 1 1 d . . . . .
O4 O 0.0065(6) 0.250000 0.6623(5) 0.0101(8) Uani 1 2 d S T P . .
O5 O 0.3930(4) 0.4331(4) 0.2798(4) 0.0130(6) Uani 1 1 d . . . . .
O6 O 0.6197(5) 0.250000 0.5395(5) 0.0114(8) Uani 1 2 d S T P A .
Ca1 Ca 0.46176(16) 0.250000 0.71296(16) 0.0152(2) Uani 1 2 d DS T P . .
O1W O 0.3616(6) 0.4291(7) 0.8918(6) 0.0385(14) Uani 0.885(9) 1 d D U . A 1
H1WA H 0.393(2) 0.398(3) 0.9882(14) 0.058 Uiso 0.885(9) 1 d DR . . A 1
H1WB H 0.264(6) 0.489(8) 0.855(3) 0.058 Uiso 0.885(9) 1 d DR . . A 1
O1B O 0.382(6) 0.250000 0.917(4) 0.087(14) Uani 0.229(18) 2 d DS TU P A 2
H1BA H 0.268679 0.250000 0.865647 0.131 Uiso 0.229(18) 2 d DRS T P A 2
H1BB H 0.420089 0.230130 1.015677 0.131 Uiso 0.115(9) 1 d DR . . 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
Ni1 O1 2.021(3) . ?
Ni1 O2 2.154(3) 3_565 ?
Ni1 O3 2.038(3) . ?
Ni1 O4 2.099(3) 3_566 ?
Ni1 O5 2.053(3) . ?
Ni1 O6 2.116(3) 3_666 ?
Se1 O1 1.695(3) 4_565 ?
Se1 O1 1.695(3) . ?
Se1 O2 1.738(4) . ?
Se2 O3 1.714(3) . ?
Se2 O3 1.714(3) 4_565 ?
Se2 O4 1.717(4) . ?
Se2 Ca1 3.1656(13) . ?
Se3 O5 1.682(3) 4_565 ?
Se3 O5 1.682(3) . ?
Se3 O6 1.735(4) . ?
O2 Ca1 2.477(4) 1_454 ?
O3 Ca1 2.486(3) . ?
O5 Ca1 2.590(3) 3_666 ?
O6 Ca1 2.355(4) . ?
Ca1 O1W 2.445(4) 4_565 ?
Ca1 O1W 2.445(4) . ?
Ca1 O1B 2.17(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
O1 Ni1 O2 92.14(12) . 3_565 ?
O1 Ni1 O3 98.68(12) . . ?
O1 Ni1 O4 90.00(13) . 3_566 ?
O1 Ni1 O5 98.22(11) . . ?
O1 Ni1 O6 166.73(12) . 3_666 ?
O3 Ni1 O2 167.72(12) . 3_565 ?
O3 Ni1 O4 91.43(12) . 3_566 ?
O3 Ni1 O5 100.45(12) . . ?
O3 Ni1 O6 92.34(13) . 3_666 ?
O4 Ni1 O2 82.72(12) 3_566 3_565 ?
O4 Ni1 O6 82.32(13) 3_566 3_666 ?
O5 Ni1 O2 83.63(12) . 3_565 ?
O5 Ni1 O4 164.30(11) . 3_566 ?
O5 Ni1 O6 86.94(12) . 3_666 ?
O6 Ni1 O2 76.22(13) 3_666 3_565 ?
O1 Se1 O1 99.21(19) . 4_565 ?
O1 Se1 O2 101.62(13) . . ?
O1 Se1 O2 101.62(13) 4_565 . ?
O3 Se2 O3 95.37(19) 4_565 . ?
O3 Se2 O4 100.03(14) 4_565 . ?
O3 Se2 O4 100.03(14) . . ?
O3 Se2 Ca1 51.34(10) 4_565 . ?
O3 Se2 Ca1 51.34(10) . . ?
O4 Se2 Ca1 83.11(14) . . ?
O5 Se3 O5 106.7(2) 4_565 . ?
O5 Se3 O6 101.56(13) 4_565 . ?
O5 Se3 O6 101.56(13) . . ?
Se1 O1 Ni1 119.51(15) . . ?
Ni1 O2 Ni1 81.96(14) 2_545 3_565 ?
Ni1 O2 Ca1 89.05(12) 3_565 1_454 ?
Ni1 O2 Ca1 89.05(12) 2_545 1_454 ?
Se1 O2 Ni1 112.85(15) . 3_565 ?
Se1 O2 Ni1 112.85(15) . 2_545 ?
Se1 O2 Ca1 150.3(2) . 1_454 ?
Ni1 O3 Ca1 125.84(13) . . ?
Se2 O3 Ni1 115.89(16) . . ?
Se2 O3 Ca1 96.09(12) . . ?
Ni1 O4 Ni1 84.57(14) 2_546 3_566 ?
Se2 O4 Ni1 116.14(16) . 3_566 ?
Se2 O4 Ni1 116.14(16) . 2_546 ?
Ni1 O5 Ca1 88.26(10) . 3_666 ?
Se3 O5 Ni1 144.27(17) . . ?
Se3 O5 Ca1 118.83(14) . 3_666 ?
Ni1 O6 Ni1 83.75(15) 3_666 2_646 ?
Ni1 O6 Ca1 93.31(13) 3_666 . ?
Ni1 O6 Ca1 93.31(13) 2_646 . ?
Se3 O6 Ni1 121.88(15) . 2_646 ?
Se3 O6 Ni1 121.88(15) . 3_666 ?
Se3 O6 Ca1 130.4(2) . . ?
Ni1 Ca1 Ni1 51.42(3) 3_666 2_646 ?
Se2 Ca1 Ni1 132.39(4) . 3_666 ?
Se2 Ca1 Ni1 132.39(4) . 2_646 ?
O2 Ca1 Ni1 41.41(7) 1_656 2_646 ?
O2 Ca1 Ni1 41.41(7) 1_656 3_666 ?
O2 Ca1 Se2 172.09(10) 1_656 . ?
O2 Ca1 O3 144.19(8) 1_656 4_565 ?
O2 Ca1 O3 144.19(8) 1_656 . ?
O2 Ca1 O5 67.21(7) 1_656 3_666 ?
O2 Ca1 O5 67.21(7) 1_656 2_646 ?
O3 Ca1 Ni1 133.31(8) 4_565 3_666 ?
O3 Ca1 Ni1 104.10(7) 4_565 2_646 ?
O3 Ca1 Ni1 133.31(8) . 2_646 ?
O3 Ca1 Ni1 104.10(7) . 3_666 ?
O3 Ca1 Se2 32.57(6) 4_565 . ?
O3 Ca1 Se2 32.57(6) . . ?
O3 Ca1 O3 61.30(13) 4_565 . ?
O3 Ca1 O5 78.46(9) . 3_666 ?
O3 Ca1 O5 78.46(9) 4_565 2_646 ?
O3 Ca1 O5 136.05(11) . 2_646 ?
O3 Ca1 O5 136.05(11) 4_565 3_666 ?
O5 Ca1 Ni1 39.08(6) 3_666 3_666 ?
O5 Ca1 Ni1 39.08(6) 2_646 2_646 ?
O5 Ca1 Ni1 90.38(7) 3_666 2_646 ?
O5 Ca1 Ni1 90.38(7) 2_646 3_666 ?
O5 Ca1 Se2 110.96(7) 3_666 . ?
O5 Ca1 Se2 110.96(7) 2_646 . ?
O5 Ca1 O5 128.95(13) 3_666 2_646 ?
O6 Ca1 Ni1 40.45(7) . 2_646 ?
O6 Ca1 Ni1 40.45(7) . 3_666 ?
O6 Ca1 Se2 106.06(11) . . ?
O6 Ca1 O2 66.03(14) . 1_656 ?
O6 Ca1 O3 93.84(11) . 4_565 ?
O6 Ca1 O3 93.84(11) . . ?
O6 Ca1 O5 70.74(7) . 2_646 ?
O6 Ca1 O5 70.74(7) . 3_666 ?
O6 Ca1 O1W 146.38(12) . 4_565 ?
O6 Ca1 O1W 146.38(12) . . ?
O1W Ca1 Ni1 144.05(12) 4_565 3_666 ?
O1W Ca1 Ni1 144.05(12) . 2_646 ?
O1W Ca1 Ni1 109.92(12) 4_565 2_646 ?
O1W Ca1 Ni1 109.92(12) . 3_666 ?
O1W Ca1 Se2 83.46(12) 4_565 . ?
O1W Ca1 Se2 83.46(12) . . ?
O1W Ca1 O2 103.15(14) 4_565 1_656 ?
O1W Ca1 O2 103.15(14) . 1_656 ?
O1W Ca1 O3 108.88(14) 4_565 . ?
O1W Ca1 O3 108.88(14) . 4_565 ?
O1W Ca1 O3 76.87(14) 4_565 4_565 ?
O1W Ca1 O3 76.87(13) . . ?
O1W Ca1 O5 136.77(14) 4_565 3_666 ?
O1W Ca1 O5 75.73(14) . 3_666 ?
O1W Ca1 O5 136.76(14) . 2_646 ?
O1W Ca1 O5 75.73(14) 4_565 2_646 ?
O1W Ca1 O1W 65.4(2) . 4_565 ?
O1B Ca1 Se2 87.4(10) . . ?
O1B Ca1 O3 97.8(9) . . ?
O1B Ca1 O6 166.5(10) . . ?
O1B Ca1 O1W 33.07(19) . 4_565 ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.557
_oxdiff_exptl_absorpt_empirical_full_min 0.754
_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_cani2(seo3)3
_database_code_depnum_ccdc_archive 'CCDC 2056696'
loop_
_audit_author_name
_audit_author_address
'xing huang'
;Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences
China
;
_audit_update_record             
;
2021-01-17 deposited with the CCDC.	2021-03-11 downloaded from the CCDC.
;
_audit_creation_date             2020-07-17
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        CaNi2(SeO3)3
_chemical_formula_moiety         '0.25(Ca4 Ni8 O36 Se12)'
_chemical_formula_sum            'Ca Ni2 O9 Se3'
_chemical_formula_weight         538.38
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ca Ca 0.2262 0.3064 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 '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           63
_space_group_name_H-M_alt        'C m c m'
_space_group_name_Hall           '-C 2c 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y, -z-1/2'
'x, -y, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z-1/2'
'x+1/2, -y+1/2, z-1/2'
'-x+1/2, y+1/2, z'

_cell_length_a                   7.3759(3)
_cell_length_b                   10.9715(5)
_cell_length_c                   10.2189(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     826.96(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3405
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      32.9380
_cell_measurement_theta_min      3.2750
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    18.406
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58348
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46c (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_colour_modifier   ?
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    4.324
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0398
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4259
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.207
_diffrn_reflns_theta_min         3.328
_diffrn_ambient_temperature      297
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -118.00  62.00   0.50    5.00    --  -28.00  45.00 180.00  360
  2  ω   -118.00  22.00   0.50    5.00    --  -28.00  45.00  90.00  280
  3  ω   -118.00 -38.00   0.50    5.00    --  -28.00  45.00   0.00  160
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0778513000
_diffrn_orient_matrix_UB_12      0.0052965000
_diffrn_orient_matrix_UB_13      0.0402877000
_diffrn_orient_matrix_UB_21      -0.0563328000
_diffrn_orient_matrix_UB_22      -0.0017990000
_diffrn_orient_matrix_UB_23      -0.0562528000
_diffrn_orient_matrix_UB_31      -0.0049731000
_diffrn_orient_matrix_UB_32      -0.0644173000
_diffrn_orient_matrix_UB_33      0.0047946000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                792
_reflns_number_total             845
_reflns_odcompleteness_completeness 95.36
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     33.13
_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       'CrysAlisPro 1.171.39.46c (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46c (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46c (Rigaku OD, 2018)'
_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, 2015)'
_refine_diff_density_max         1.277
_refine_diff_density_min         -0.836
_refine_diff_density_rms         0.204
_refine_ls_extinction_coef       0.0014(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     49
_refine_ls_number_reflns         845
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0261
_refine_ls_restrained_S_all      1.147
_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)+(0.0329P)²+3.9566P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0687
_refine_ls_wR_factor_ref         0.0697
_refine_special_details          ?
_olex2_refinement_description    
;
1. Others
 Fixed Sof: Se2(0.25)
;
_atom_sites_solution_hydrogens   .
_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
Se1 Se 0.500000 0.23695(4) 0.52997(3) 0.00928(13) Uani 1 2 d S T P . .
Ni1 Ni 0.19086(6) 0.25418(4) 0.750000 0.00731(13) Uani 1 2 d S T P . .
Se2 Se 0.500000 0.48617(7) 0.81732(7) 0.00853(16) Uani 0.5 2 d S T P . .
Ca1 Ca 0.500000 -0.01931(10) 0.250000 0.0122(2) Uani 1 4 d S T P . .
O1 O 0.500000 0.1647(2) 0.3802(3) 0.0095(5) Uani 1 2 d S T P . .
O2 O 0.3281(3) 0.16337(19) 0.60735(19) 0.0124(4) Uani 1 1 d . . . . .
O3 O 0.3180(4) 0.4185(3) 0.750000 0.0156(6) Uani 1 2 d S T P . .
O4 O 0.500000 0.6208(4) 0.750000 0.0203(9) Uani 1 4 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
Se1 Ca1 3.2799(9) 9_656 ?
Se1 O1 1.723(3) . ?
Se1 O2 1.6984(19) 12_655 ?
Se1 O2 1.6983(19) . ?
Ni1 O1 2.132(2) 13_556 ?
Ni1 O1 2.132(2) 6 ?
Ni1 O2 2.035(2) 10_557 ?
Ni1 O2 2.035(2) . ?
Ni1 O3 2.032(3) . ?
Ni1 O4 2.030(3) 5_445 ?
Se2 Se2 1.3759(14) 10_557 ?
Se2 O3 1.681(3) 3_656 ?
Se2 O3 1.681(3) . ?
Se2 O4 1.630(4) . ?
Ca1 O1 2.418(3) . ?
Ca1 O1 2.418(3) 10_556 ?
Ca1 O2 2.496(2) 4_556 ?
Ca1 O2 2.496(2) 9_656 ?
Ca1 O2 2.496(2) 2_654 ?
Ca1 O2 2.496(2) 11 ?
Ca1 O3 2.593(3) 15 ?
Ca1 O3 2.593(3) 13_556 ?

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 Se1 Ca1 105.89(9) . 9_656 ?
O2 Se1 Ca1 48.30(7) . 9_656 ?
O2 Se1 Ca1 48.30(7) 12_655 9_656 ?
O2 Se1 O1 101.23(10) . . ?
O2 Se1 O1 101.23(10) 12_655 . ?
O2 Se1 O2 96.58(14) . 12_655 ?
O1 Ni1 O1 77.25(12) 13_556 6 ?
O2 Ni1 O1 94.92(9) . 13_556 ?
O2 Ni1 O1 94.92(9) 10_557 6 ?
O2 Ni1 O1 168.50(8) 10_557 13_556 ?
O2 Ni1 O1 168.50(8) . 6 ?
O2 Ni1 O2 91.49(12) 10_557 . ?
O3 Ni1 O1 86.24(9) . 6 ?
O3 Ni1 O1 86.24(9) . 13_556 ?
O3 Ni1 O2 101.81(8) . 10_557 ?
O3 Ni1 O2 101.81(8) . . ?
O4 Ni1 O1 80.97(9) 5_445 6 ?
O4 Ni1 O1 80.97(9) 5_445 13_556 ?
O4 Ni1 O2 89.55(8) 5_445 10_557 ?
O4 Ni1 O2 89.55(8) 5_445 . ?
O4 Ni1 O3 163.59(12) 5_445 . ?
Se2 Se2 O3 65.84(4) 10_557 . ?
Se2 Se2 O3 65.84(4) 10_557 3_656 ?
Se2 Se2 O4 65.03(7) 10_557 . ?
O3 Se2 O3 105.96(17) . 3_656 ?
O4 Se2 O3 103.15(10) . 3_656 ?
O4 Se2 O3 103.15(10) . . ?
Se1 Ca1 Se1 86.56(3) 2_654 9_656 ?
Ni1 Ca1 Se1 130.944(10) 13_556 2_654 ?
Ni1 Ca1 Se1 130.944(10) 13_556 9_656 ?
Ni1 Ca1 Se1 130.944(10) 15 2_654 ?
Ni1 Ca1 Se1 130.944(10) 15 9_656 ?
Ni1 Ca1 Ni1 51.65(2) 15 13_556 ?
O1 Ca1 Se1 170.12(7) 10_556 9_656 ?
O1 Ca1 Se1 103.33(6) . 9_656 ?
O1 Ca1 Se1 170.12(7) . 2_654 ?
O1 Ca1 Se1 103.32(6) 10_556 2_654 ?
O1 Ca1 Ni1 41.28(5) 10_556 13_556 ?
O1 Ca1 Ni1 41.28(5) 10_556 15 ?
O1 Ca1 Ni1 41.28(5) . 15 ?
O1 Ca1 Ni1 41.28(5) . 13_556 ?
O1 Ca1 O1 66.79(13) 10_556 . ?
O1 Ca1 O2 101.96(7) . 4_556 ?
O1 Ca1 O2 101.96(7) 10_556 2_654 ?
O1 Ca1 O2 148.22(5) . 2_654 ?
O1 Ca1 O2 101.96(7) 10_556 11 ?
O1 Ca1 O2 148.22(5) 10_556 9_656 ?
O1 Ca1 O2 148.22(5) . 11 ?
O1 Ca1 O2 101.96(7) . 9_656 ?
O1 Ca1 O2 148.22(5) 10_556 4_556 ?
O1 Ca1 O3 69.15(6) . 13_556 ?
O1 Ca1 O3 69.15(6) . 15 ?
O1 Ca1 O3 69.15(6) 10_556 15 ?
O1 Ca1 O3 69.15(6) 10_556 13_556 ?
O2 Ca1 Se1 86.52(5) 4_556 2_654 ?
O2 Ca1 Se1 30.53(4) 11 2_654 ?
O2 Ca1 Se1 30.53(4) 9_656 9_656 ?
O2 Ca1 Se1 30.53(4) 2_654 2_654 ?
O2 Ca1 Se1 86.52(5) 9_656 2_654 ?
O2 Ca1 Se1 86.52(5) 2_654 9_656 ?
O2 Ca1 Se1 30.53(4) 4_556 9_656 ?
O2 Ca1 Se1 86.52(5) 11 9_656 ?
O2 Ca1 Ni1 110.41(5) 11 13_556 ?
O2 Ca1 Ni1 142.30(5) 4_556 15 ?
O2 Ca1 Ni1 110.41(5) 9_656 15 ?
O2 Ca1 Ni1 110.41(5) 4_556 13_556 ?
O2 Ca1 Ni1 110.41(5) 2_654 15 ?
O2 Ca1 Ni1 142.30(5) 2_654 13_556 ?
O2 Ca1 Ni1 142.30(5) 9_656 13_556 ?
O2 Ca1 Ni1 142.30(5) 11 15 ?
O2 Ca1 O2 61.05(9) 11 2_654 ?
O2 Ca1 O2 71.46(9) 11 4_556 ?
O2 Ca1 O2 101.42(10) 4_556 2_654 ?
O2 Ca1 O2 101.42(10) 11 9_656 ?
O2 Ca1 O2 61.05(9) 4_556 9_656 ?
O2 Ca1 O2 71.46(9) 2_654 9_656 ?
O2 Ca1 O3 136.84(6) 11 15 ?
O2 Ca1 O3 136.84(6) 9_656 13_556 ?
O2 Ca1 O3 79.08(7) 2_654 15 ?
O2 Ca1 O3 79.08(7) 11 13_556 ?
O2 Ca1 O3 136.84(6) 4_556 15 ?
O2 Ca1 O3 79.08(7) 4_556 13_556 ?
O2 Ca1 O3 79.08(7) 9_656 15 ?
O2 Ca1 O3 136.84(6) 2_654 13_556 ?
O3 Ca1 Se1 108.08(4) 15 9_656 ?
O3 Ca1 Se1 108.08(4) 13_556 2_654 ?
O3 Ca1 Se1 108.08(4) 15 2_654 ?
O3 Ca1 Se1 108.08(4) 13_556 9_656 ?
O3 Ca1 Ni1 38.94(6) 13_556 13_556 ?
O3 Ca1 Ni1 38.94(6) 15 15 ?
O3 Ca1 Ni1 90.59(7) 15 13_556 ?
O3 Ca1 Ni1 90.59(7) 13_556 15 ?
O3 Ca1 O3 129.52(13) 15 13_556 ?
Se1 O1 Ni1 111.23(11) . 13_556 ?
Se1 O1 Ni1 111.23(11) . 15 ?
Se1 O1 Ca1 150.79(15) . . ?
Ni1 O1 Ni1 82.65(10) 13_556 15 ?
Ni1 O1 Ca1 90.28(8) 15 . ?
Ni1 O1 Ca1 90.28(8) 13_556 . ?
Se1 O2 Ni1 118.17(11) . . ?
Se1 O2 Ca1 101.17(9) . 9_656 ?
Ni1 O2 Ca1 98.30(8) . 9_656 ?
Ni1 O3 Ca1 87.75(10) . 13_556 ?
Se2 O3 Ni1 139.48(14) 10_557 . ?
Se2 O3 Ni1 139.49(14) . . ?
Se2 O3 Se2 48.32(9) 10_557 . ?
Se2 O3 Ca1 122.27(14) 10_557 13_556 ?
Se2 O3 Ca1 122.27(14) . 13_556 ?
Ni1 O4 Ni1 87.80(17) 5 7_556 ?
Se2 O4 Ni1 130.79(5) 10_557 7_556 ?
Se2 O4 Ni1 130.79(5) . 5 ?
Se2 O4 Ni1 130.79(5) . 7_556 ?
Se2 O4 Ni1 130.79(5) 10_557 5 ?
Se2 O4 Se2 49.93(13) . 10_557 ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.005
_oxdiff_exptl_absorpt_empirical_full_min 0.738
_exptl_crystal_preparation       'Magnetic properties'
