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_7708871
_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         '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  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w   -118.00  62.00   0.50    5.00    --  -28.00  45.00 180.00  360
  2  \w   -118.00  22.00   0.50    5.00    --  -28.00  45.00  90.00  280
  3  \w   -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       '\w 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/[\s^2^(Fo^2^)+(0.0387P)^2^+0.1466P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(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
_reflns_odcompleteness_completeness 82.59
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     33.24
_olex2_refinement_description
;
;
_shelx_res_checksum              20849
_shelx_hkl_checksum              90778
_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