#------------------------------------------------------------------------------
#$Date: 2021-11-19 01:58:33 +0200 (Fri, 19 Nov 2021) $
#$Revision: 270753 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/88/7708871.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_7708871
loop_
_publ_author_name
'Huang, Xing'
'Zhao, Zhiying'
'Wang, Yanqi'
'Zhang, Mengsi'
'He, Zhangzhen'
_publ_section_title
;
 Synthesis, structure and magnetic properties of two new spin-chain
 compounds Ca2Ni(HSeO3)2(SeO3)2 and Na2Cu(SeO3)2·2H2O
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03058B
_journal_year                    2021
_chemical_formula_moiety         'Ca2 H2 Ni O12 Se4'
_chemical_formula_sum            'Ca2 H2 Ni O12 Se4'
_chemical_formula_weight         648.73
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2020-06-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                110.413(3)
_cell_angle_beta                 105.027(3)
_cell_angle_gamma                91.786(2)
_cell_formula_units_Z            1
_cell_length_a                   5.2858(2)
_cell_length_b                   7.0398(2)
_cell_length_c                   8.4180(3)
_cell_measurement_reflns_used    2509
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.9330
_cell_measurement_theta_min      2.6520
_cell_volume                     280.962(18)
_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)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.826
_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      -0.1292324000
_diffrn_orient_matrix_UB_12      0.0275541000
_diffrn_orient_matrix_UB_13      -0.0069755000
_diffrn_orient_matrix_UB_21      0.0164638000
_diffrn_orient_matrix_UB_22      0.0500853000
_diffrn_orient_matrix_UB_23      -0.0573052000
_diffrn_orient_matrix_UB_31      -0.0518362000
_diffrn_orient_matrix_UB_32      -0.0922076000
_diffrn_orient_matrix_UB_33      -0.0740518000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0147
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.826
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3058
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.826
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.320
_diffrn_reflns_theta_min         2.696
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    15.654
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63441
_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            greenish
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_density_diffrn    3.834
_exptl_crystal_description       block
_exptl_crystal_F_000             302
_refine_diff_density_max         0.742
_refine_diff_density_min         -1.209
_refine_diff_density_rms         0.223
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     92
_refine_ls_number_reflns         1789
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0281
_refine_ls_R_factor_gt           0.0256
_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)+(0.0387P)²+0.1466P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0636
_refine_ls_wR_factor_ref         0.0650
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1651
_reflns_number_total             1789
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1dt03058b1.cif
_cod_data_source_block           ca2ni(hseo3)2(seo3)2
_cod_database_code               7708871
_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 82.59
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     33.24
_olex2_refinement_description
;
;
_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 1.795
_oxdiff_exptl_absorpt_empirical_full_min 0.587
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -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
Se1 Se -0.07065(5) 0.23864(4) 0.31915(3) 0.00761(8) Uani 1 1 d . . . . .
Se2 Se 0.70857(5) 0.18973(4) 0.72458(3) 0.00950(8) Uani 1 1 d . . . . .
Ni1 Ni 0.500000 0.500000 0.500000 0.00764(11) Uani 1 2 d S T P . .
Ca1 Ca 0.38290(10) 0.27180(9) 0.04715(7) 0.00887(12) Uani 1 1 d . . . . .
O1 O 0.6350(4) 0.3716(3) 0.8885(3) 0.0137(4) Uani 1 1 d . . . . .
O2 O -0.2517(4) 0.4395(3) 0.3333(3) 0.0105(4) Uani 1 1 d . . . . .
O3 O 0.1953(4) 0.3298(3) 0.2763(3) 0.0108(4) Uani 1 1 d . . . . .
O4 O 0.5771(4) 0.2353(3) 0.5427(3) 0.0136(4) Uani 1 1 d . . . . .
O5 O 1.0545(4) 0.2704(4) 0.7739(3) 0.0155(4) Uani 1 1 d . . . . .
O6 O -0.2516(4) 0.0782(3) 0.1167(3) 0.0146(4) Uani 1 1 d . . . . .
H5 H 1.096(12) 0.366(9) 0.740(9) 0.065(19) Uiso 1 1 d . . . . .
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
O2 Se1 Ca1 50.07(7) . 1_455 ?
O3 Se1 Ca1 110.41(7) . 1_455 ?
O3 Se1 O2 99.97(10) . . ?
O6 Se1 Ca1 47.67(8) . 1_455 ?
O6 Se1 O2 97.58(10) . . ?
O6 Se1 O3 102.40(10) . . ?
O1 Se2 Ca1 36.78(8) . 1_556 ?
O1 Se2 O5 100.58(11) . . ?
O4 Se2 Ca1 120.73(8) . 1_556 ?
O4 Se2 O1 106.37(11) . . ?
O4 Se2 O5 103.12(11) . . ?
O5 Se2 Ca1 123.28(7) . 1_556 ?
O2 Ni1 O2 180.0 2_566 1_655 ?
O3 Ni1 O2 86.65(8) . 1_655 ?
O3 Ni1 O2 86.65(8) 2_666 2_566 ?
O3 Ni1 O2 93.35(8) 2_666 1_655 ?
O3 Ni1 O2 93.35(8) . 2_566 ?
O3 Ni1 O3 180.00(9) . 2_666 ?
O4 Ni1 O2 89.04(8) . 1_655 ?
O4 Ni1 O2 89.04(8) 2_666 2_566 ?
O4 Ni1 O2 90.96(8) 2_666 1_655 ?
O4 Ni1 O2 90.96(8) . 2_566 ?
O4 Ni1 O3 91.30(8) . 2_666 ?
O4 Ni1 O3 88.70(8) . . ?
O4 Ni1 O3 88.70(8) 2_666 2_666 ?
O4 Ni1 O3 91.30(8) 2_666 . ?
O4 Ni1 O4 180.0 2_666 . ?
Se1 Ca1 Se2 88.957(15) 1_655 1_554 ?
Se1 Ca1 Ni1 58.966(10) 1_655 . ?
Se1 Ca1 Ca1 62.844(15) 1_655 2_655 ?
Se1 Ca1 Ca1 99.47(2) 1_655 2_665 ?
Se2 Ca1 Ca1 72.255(16) 1_554 2_655 ?
Se2 Ca1 Ca1 61.141(15) 1_554 2_665 ?
Ni1 Ca1 Se2 140.541(17) . 1_554 ?
Ni1 Ca1 Ca1 99.38(2) . 2_665 ?
Ni1 Ca1 Ca1 106.92(2) . 2_655 ?
Ca1 Ca1 Ca1 130.63(3) 2_665 2_655 ?
O1 Ca1 Se1 89.16(6) 1_554 1_655 ?
O1 Ca1 Se1 106.08(6) 2_666 1_655 ?
O1 Ca1 Se2 97.22(5) 2_666 1_554 ?
O1 Ca1 Se2 24.98(5) 1_554 1_554 ?
O1 Ca1 Ni1 73.36(5) 2_666 . ?
O1 Ca1 Ni1 123.54(6) 1_554 . ?
O1 Ca1 Ca1 164.14(6) 2_666 2_655 ?
O1 Ca1 Ca1 36.83(5) 1_554 2_665 ?
O1 Ca1 Ca1 94.52(6) 1_554 2_655 ?
O1 Ca1 Ca1 36.36(5) 2_666 2_665 ?
O1 Ca1 O1 73.19(8) 1_554 2_666 ?
O1 Ca1 O2 91.05(7) 1_554 1_655 ?
O1 Ca1 O2 76.64(7) 2_666 1_655 ?
O1 Ca1 O5 74.80(8) 1_554 1_454 ?
O1 Ca1 O5 78.05(8) 2_666 1_454 ?
O1 Ca1 O6 84.69(8) 1_554 1_655 ?
O1 Ca1 O6 132.26(8) 2_666 1_655 ?
O2 Ca1 Se1 31.44(5) 1_655 1_655 ?
O2 Ca1 Se2 103.43(5) 1_655 1_554 ?
O2 Ca1 Ni1 37.37(4) 1_655 . ?
O2 Ca1 Ca1 82.33(5) 1_655 2_665 ?
O2 Ca1 Ca1 93.96(5) 1_655 2_655 ?
O3 Ca1 Se1 87.04(5) . 1_655 ?
O3 Ca1 Se2 175.91(5) . 1_554 ?
O3 Ca1 Ni1 35.69(5) . . ?
O3 Ca1 Ca1 106.54(6) . 2_655 ?
O3 Ca1 Ca1 118.75(6) . 2_665 ?
O3 Ca1 O1 83.10(8) . 2_666 ?
O3 Ca1 O1 153.91(8) . 1_554 ?
O3 Ca1 O2 72.65(7) . 1_655 ?
O3 Ca1 O5 111.24(7) . 1_454 ?
O3 Ca1 O6 104.15(8) . 1_655 ?
O3 Ca1 O6 102.80(8) . 2 ?
O5 Ca1 Se1 161.70(6) 1_454 1_655 ?
O5 Ca1 Se2 72.78(5) 1_454 1_554 ?
O5 Ca1 Ni1 137.82(6) 1_454 . ?
O5 Ca1 Ca1 108.93(6) 1_454 2_655 ?
O5 Ca1 Ca1 73.02(6) 1_454 2_665 ?
O5 Ca1 O2 153.69(8) 1_454 1_655 ?
O6 Ca1 Se1 30.38(5) 1_655 1_655 ?
O6 Ca1 Se1 98.06(5) 2 1_655 ?
O6 Ca1 Se2 72.60(6) 1_655 1_554 ?
O6 Ca1 Se2 78.59(6) 2 1_554 ?
O6 Ca1 Ni1 85.63(5) 1_655 . ?
O6 Ca1 Ni1 124.71(6) 2 . ?
O6 Ca1 Ca1 111.34(6) 1_655 2_665 ?
O6 Ca1 Ca1 135.40(6) 2 2_665 ?
O6 Ca1 Ca1 36.02(5) 2 2_655 ?
O6 Ca1 Ca1 33.98(5) 1_655 2_655 ?
O6 Ca1 O1 155.45(8) 2 2_666 ?
O6 Ca1 O1 103.29(8) 2 1_554 ?
O6 Ca1 O2 127.91(7) 2 1_655 ?
O6 Ca1 O2 61.74(7) 1_655 1_655 ?
O6 Ca1 O5 136.24(8) 1_655 1_454 ?
O6 Ca1 O5 77.62(8) 2 1_454 ?
O6 Ca1 O6 70.00(8) 2 1_655 ?
Se2 O1 Ca1 132.24(11) . 2_666 ?
Se2 O1 Ca1 118.23(12) . 1_556 ?
Ca1 O1 Ca1 106.81(8) 1_556 2_666 ?
Se1 O2 Ni1 119.31(11) . 1_455 ?
Se1 O2 Ca1 98.49(9) . 1_455 ?
Ni1 O2 Ca1 95.95(7) 1_455 1_455 ?
Se1 O3 Ni1 114.50(10) . . ?
Se1 O3 Ca1 139.89(11) . . ?
Ni1 O3 Ca1 103.82(8) . . ?
Se2 O4 Ni1 132.35(12) . . ?
Se2 O5 Ca1 122.00(11) . 1_656 ?
Se1 O6 Ca1 101.95(10) . 1_455 ?
Se1 O6 Ca1 140.46(12) . 2 ?
Ca1 O6 Ca1 110.00(8) 2 1_455 ?
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 3.2597(6) 1_455 ?
Se1 O2 1.719(2) . ?
Se1 O3 1.6989(19) . ?
Se1 O6 1.685(2) . ?
Se2 Ca1 3.4730(6) 1_556 ?
Se2 O1 1.665(2) . ?
Se2 O4 1.653(2) . ?
Se2 O5 1.793(2) . ?
Ni1 O2 2.109(2) 2_566 ?
Ni1 O2 2.109(2) 1_655 ?
Ni1 O3 2.0758(19) . ?
Ni1 O3 2.0758(19) 2_666 ?
Ni1 O4 2.051(2) . ?
Ni1 O4 2.051(2) 2_666 ?
Ca1 Ca1 3.8114(12) 2_665 ?
Ca1 Ca1 3.9361(12) 2_655 ?
Ca1 O1 2.361(2) 1_554 ?
Ca1 O1 2.387(2) 2_666 ?
Ca1 O2 2.527(2) 1_655 ?
Ca1 O3 2.311(2) . ?
Ca1 O5 2.493(2) 1_454 ?
Ca1 O6 2.463(2) 1_655 ?
Ca1 O6 2.341(2) 2 ?
