CaZn(HPO3)2 and Ba2Zn(HPO3)3 : Novel Alkaline-Earth Zincophosphites with Diversified Anionic Frameworks
Zhang, Yu; Liu, Xia; Liu, Qian-Yan; Wang, Jianhua; HU, Ting; Lin, Yan-Mei; Zhang, Jian-Han; Dalton Transactions  (2023) –; doi:10.1039/D3DT01321A

data_7713521
_publ_section_title
;
 CaZn(HPO3)2 and Ba2Zn(HPO3)3 : Novel Alkaline-Earth Zincophosphites with
 Diversified Anionic Frameworks
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01321A
_journal_year                    2023
_chemical_formula_moiety         'Ca2 H4 O12 P4 Zn2'
_chemical_formula_sum            'Ca2 H4 O12 P4 Zn2'
_chemical_formula_weight         530.81
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2022-09-13
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-05-31 deposited with the CCDC.	2023-07-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.882(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   5.4232(2)
_cell_length_b                   7.6786(3)
_cell_length_c                   14.1575(5)
_cell_measurement_reflns_used    2603
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.9270
_cell_measurement_theta_min      2.8680
_cell_volume                     589.24(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.947
_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     32.00  58.00   0.50    3.02    --   20.00  54.00-150.00   52
  2  \w    -74.00 -20.00   0.50    3.02    --   20.00  54.00  90.00  108
  3  \w      4.00  85.00   0.50    3.02    --   20.00  54.00  90.00  162
  4  \w    -69.00  80.00   0.50    3.02    --   20.00  54.00-120.00  298
  5  \w    -74.00 -42.00   0.50    3.02    --   20.00  54.00   0.00   64
  6  \w      6.00  34.00   0.50    3.02    --   20.00  54.00   0.00   56
  7  \w    -71.00 -46.00   0.50    3.02    --   20.00  54.00  30.00   50
  8  \w     67.00  92.00   0.50    3.02    --   20.00  54.00  30.00   50
  9  \w    -66.00 -39.00   0.50    3.02    --   20.00  54.00 150.00   54
 10  \w     18.00  43.00   0.50    3.02    --   20.00  54.00 150.00   50
 11  \w    -30.00  -5.00   0.50    3.02    --   20.00  54.00-150.00   50
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0033482000
_diffrn_orient_matrix_UB_12      0.0922586000
_diffrn_orient_matrix_UB_13      0.0016197000
_diffrn_orient_matrix_UB_21      0.0895573000
_diffrn_orient_matrix_UB_22      0.0038513000
_diffrn_orient_matrix_UB_23      -0.0353359000
_diffrn_orient_matrix_UB_31      -0.0953807000
_diffrn_orient_matrix_UB_32      0.0003599000
_diffrn_orient_matrix_UB_33      -0.0355355000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_unetI/netI     0.0335
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            4883
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.424
_diffrn_reflns_theta_min         3.018
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.544
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73471
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.992
_exptl_crystal_description       block
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.642
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     98
_refine_ls_number_reflns         1684
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0250
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0243P)^2^+0.0653P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0551
_refine_ls_wR_factor_ref         0.0570
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1455
_reflns_number_total             1684
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01321a2.cif
_cod_data_source_block           exp_712
_cod_database_code               7713521
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'P O Ca Cl Zn'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All H(H) groups
;
_shelx_res_checksum              28123
_shelx_hkl_checksum              93209
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.156
_oxdiff_exptl_absorpt_empirical_full_min 0.868