Crystal-to-crystal transformation of a new selenite compound CaNi2(SeO3)3·2H2O induced by dehydration
Huang, Xing; Zhao, Zhiying; Zhang, Mengsi; He, Zhangzhen; CrystEngComm 23 (2021) 3126–3132; doi:10.1039/D1CE00190F

data_7242585
_publ_section_title
;
 Crystal-to-crystal transformation of a new selenite compound
 CaNi2(SeO3)3&#x00B7;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         '0.25(Ca4 Ni8 O36 Se12)'
_chemical_formula_sum            'Ca Ni2 O9 Se3'
_chemical_formula_weight         538.38
_chemical_name_systematic        CaNi2(SeO3)3
_space_group_crystal_system      orthorhombic
_space_group_IT_number           63
_space_group_name_Hall           '-C 2c 2'
_space_group_name_H-M_alt        'C m c m'
_atom_sites_solution_primary     dual
_audit_creation_date             2020-07-17
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.3759(3)
_cell_length_b                   10.9715(5)
_cell_length_c                   10.2189(3)
_cell_measurement_reflns_used    3405
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      32.9380
_cell_measurement_theta_min      3.2750
_cell_volume                     826.96(6)
_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      297
_diffrn_detector                 'CCD plate'
_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  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      -0.0778513000
_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_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_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_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_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    4.324
_exptl_crystal_description       block
_exptl_crystal_F_000             1000
_exptl_crystal_preparation       'Magnetic properties'
_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+0.001xFc^2^\l^3^/sin(2\q)]^-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_restrained_S_all      1.147
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0261
_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^)+(0.0329P)^2^+3.9566P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0687
_refine_ls_wR_factor_ref         0.0697
_reflns_Friedel_coverage         0.000
_reflns_number_gt                792
_reflns_number_total             845
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00190f2.cif
_cod_data_source_block           cani2(seo3)3
_cod_depositor_comments
'Adding full bibliography for 7242583--7242585.cif.'
_cod_database_code               7242585
_shelx_shelxl_version_number     2016/6
_reflns_odcompleteness_completeness 95.36
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     33.13
_olex2_refinement_description
;
1. Others
 Fixed Sof: Se2(0.25)
;
_shelx_res_checksum              30747
_shelx_hkl_checksum              57023
_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