Cd2(IO3)(PO4) and Cd1.62Mg0.38(IO3)(PO4): Metal iodate-phosphates with large SHG responses and wide band gaps
Chen, Qian-Qian; Hu, Chun-Li; Yao, Li-Jia; Chen, Jin; Cao, Ming-Yang; Li, Bing-Xuan; Mao, Jiang-Gao; Chemical Communications  (2022) –; doi:10.1039/D2CC02353A

data_7130221
_publ_section_title
;
 Cd2(IO3)(PO4) and Cd1.62Mg0.38(IO3)(PO4): Metal iodate-phosphates with
 large SHG responses and wide band gaps
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC02353A
_journal_year                    2022
_chemical_formula_moiety         'Cd1.623 I Mg0.377 O7 P'
_chemical_formula_sum            'Cd1.62 I Mg0.38 O7 P'
_chemical_formula_weight         461.47
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-05-21
_audit_creation_method
;
Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6429)
;
_audit_update_record
;
2022-05-22 deposited with the CCDC.	2022-06-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   15.3319(13)
_cell_length_b                   12.2073(11)
_cell_length_c                   12.2169(16)
_cell_measurement_reflns_used    2428
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.0640
_cell_measurement_theta_min      2.6440
_cell_volume                     2286.5(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.3468
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.953
_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    -60.00  35.00   1.00    1.09    --   10.53 -57.00 -90.00   95
  2  \w    -18.00  84.00   1.00    1.09    --   10.53  57.00  60.00  102
  3  \w    -68.00  15.00   1.00    1.09    --  -11.16 -57.00 120.00   83
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0473
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4515
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.467
_diffrn_reflns_theta_min         2.657
_exptl_absorpt_coefficient_mu    11.782
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.600
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.115a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    5.362
_exptl_crystal_description       Blocky
_exptl_crystal_F_000             3303
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.988
_refine_diff_density_min         -2.467
_refine_diff_density_rms         0.376
_refine_ls_abs_structure_details
;
 Twinning involves inversion, so Flack parameter cannot be determined
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     105
_refine_ls_number_reflns         1339
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0354
_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^)+(0.0373P)^2^+119.6597P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0779
_refine_ls_wR_factor_ref         0.0794
_reflns_Friedel_coverage         0.913
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.950
_reflns_number_gt                1302
_reflns_number_total             1339
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc02353a2.cif
_cod_data_source_block           2
_cod_database_code               7130221
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.271
_shelx_estimated_absorpt_t_min   0.172
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.36(13)
 0.05(7) 0.14(8) 0.45(7)
2. Shared sites
{Cd2, Mg1}
3. Uiso/Uaniso restraints and constraints
Uanis(O7) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O4) \\sim
Ueq, Uanis(O3) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O6) \\sim Ueq: with sigma
of 0.003 and sigma for terminal atoms of 0.006
Uanis(Cd2) = Uanis(Mg1)
4. Others
 Sof(Mg1)=0.5*(1-FVAR(2))
 Sof(Cd2)=0.5*FVAR(2)
;
_shelx_res_checksum              25226
_shelx_hkl_checksum              82250
_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
;