#------------------------------------------------------------------------------
#$Date: 2021-06-05 21:06:51 +0300 (Sat, 05 Jun 2021) $
#$Revision: 265938 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/25/7242584.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7242584
loop_
_publ_author_name
'Huang, Xing'
'Zhao, Zhiying'
'Zhang, Mengsi'
'He, Zhangzhen'
_publ_section_title
;
 Crystal-to-crystal transformation of a new selenite compound
 CaNi2(SeO3)3·2H2O induced by dehydration
;
_journal_issue                   17
_journal_name_full               CrystEngComm
_journal_page_first              3126
_journal_page_last               3132
_journal_paper_doi               10.1039/D1CE00190F
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         '0.5(Ca2 H8 Ni4 O22 Se6)'
_chemical_formula_sum            'Ca H4 Ni2 O11 Se3'
_chemical_formula_weight         574.41
_chemical_name_systematic        CaNi2(SeO3)3(2H2O)
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_date             2020-09-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-01-17 deposited with the CCDC.	2021-03-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.275(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.8568(4)
_cell_length_b                   7.3734(3)
_cell_length_c                   8.9697(6)
_cell_measurement_reflns_used    2666
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      33.0000
_cell_measurement_theta_min      2.4730
_cell_volume                     473.68(5)
_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)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_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_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_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_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_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    4.027
_exptl_crystal_description       needle
_exptl_crystal_F_000             540
_exptl_crystal_preparation       'Magnetic properties'
_refine_diff_density_max         1.222
_refine_diff_density_min         -1.316
_refine_diff_density_rms         0.259
_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_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_gt           0.0358
_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
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1439
_reflns_number_total             1802
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1ce00190f2.cif
_cod_data_source_block           x_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7242583--7242585.cif.'
_cod_database_code               7242584
_shelx_shelxl_version_number     2016/6
_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.
;
_reflns_odcompleteness_completeness 94.26
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     32.97
_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)
;
_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
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'
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
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'
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 ?
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) . ?
