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_7242584
_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         '0.5(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  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  25.00   0.50    5.00    --  -25.00  45.00  90.00  280
  3  \w   -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       '\w 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/[\s^2^(Fo^2^)+(0.0269P)^2^+0.7444P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(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
_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)
;
_shelx_res_checksum              26303
_shelx_hkl_checksum              78149
_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