Synthesis, structure and magnetic properties of two new spin-chain compounds Ca2Ni(HSeO3)2(SeO3)2 and Na2Cu(SeO3)2·2H2O
Huang, Xing; Zhao, Zhiying; Wang, Yanqi; Zhang, Mengsi; He, Zhangzhen; Dalton Transactions  (2021) –; doi:10.1039/D1DT03058B

data_7708870
_publ_section_title
;
 Synthesis, structure and magnetic properties of two new spin-chain
 compounds Ca2Ni(HSeO3)2(SeO3)2 and Na2Cu(SeO3)2&#x00B7;2H2O
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03058B
_journal_year                    2021
_chemical_formula_moiety         'Cu H4 Na2 O8 Se2'
_chemical_formula_sum            'Cu H4 Na2 O8 Se2'
_chemical_formula_weight         399.47
_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             2021-04-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                103.914(2)
_cell_angle_beta                 104.661(2)
_cell_angle_gamma                105.325(2)
_cell_formula_units_Z            1
_cell_length_a                   5.19270(10)
_cell_length_b                   5.9081(2)
_cell_length_c                   7.5358(2)
_cell_measurement_reflns_used    2795
_cell_measurement_temperature    293
_cell_measurement_theta_max      32.7600
_cell_measurement_theta_min      3.7590
_cell_volume                     203.670(11)
_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 0.992
_diffrn_measured_fraction_theta_max 0.924
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w   -115.00  65.00   0.50    5.00    --  -25.00  45.00   0.00  360
  2  \w   -115.00  65.00   0.50    5.00    --  -25.00  45.00  90.00  360
  3  \w   -115.00  65.00   0.50    5.00    --  -25.00  45.00 180.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0712795000
_diffrn_orient_matrix_UB_12      -0.0495073000
_diffrn_orient_matrix_UB_13      0.0658853000
_diffrn_orient_matrix_UB_21      -0.1247278000
_diffrn_orient_matrix_UB_22      -0.1055324000
_diffrn_orient_matrix_UB_23      -0.0306817000
_diffrn_orient_matrix_UB_31      0.0448667000
_diffrn_orient_matrix_UB_32      -0.0615929000
_diffrn_orient_matrix_UB_33      -0.0730462000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_av_unetI/netI     0.0216
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.924
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3242
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.924
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.140
_diffrn_reflns_theta_min         2.959
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    11.732
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60210
_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            bluish
_exptl_crystal_colour_modifier   bluish
_exptl_crystal_density_diffrn    3.257
_exptl_crystal_description       prism
_exptl_crystal_F_000             187
_refine_diff_density_max         0.510
_refine_diff_density_min         -1.084
_refine_diff_density_rms         0.197
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     69
_refine_ls_number_reflns         1425
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0210
_refine_ls_R_factor_gt           0.0192
_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/[\s^2^(Fo^2^)+(0.0256P)^2^+0.0105P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0428
_refine_ls_wR_factor_ref         0.0433
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1362
_reflns_number_total             1425
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03058b2.cif
_cod_data_source_block           nacuseo
_cod_original_cell_volume        203.670(10)
_cod_database_code               7708870
_shelx_shelxl_version_number     2016/6
_reflns_odcompleteness_completeness 92.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     33.06
_olex2_refinement_description
;
;
_shelx_res_checksum              14609
_shelx_hkl_checksum              64047
_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 2.458
_oxdiff_exptl_absorpt_empirical_full_min 0.667