KMg(H2O)PO4: A Deep-Ultraviolet Transparent Nonlinear Optical Material Derived from KTiOPO4
Bai, Zhiyong; Hu, Chun-Li; Liu, Lehui; Zhang, Lizhen; Huang, Yisheng; Yuan, Feifei; Lin, Zhoubin; Chemistry of Materials 31 (2019) 9540–; doi:10.1021/acs.chemmater.9b03950

data_4003140
_publ_section_title
;
 KMg(H2O)PO4: A Deep-Ultraviolet Transparent Nonlinear Optical Material
 Derived from KTiOPO4
;
_journal_issue                   22
_journal_name_full               'Chemistry of Materials'
_journal_page_first              9540
_journal_paper_doi               10.1021/acs.chemmater.9b03950
_journal_volume                  31
_journal_year                    2019
_chemical_formula_moiety         '0.5(H4 K2 Mg2 O10 P2)'
_chemical_formula_sum            'H2 K Mg O5 P'
_chemical_formula_weight         176.40
_space_group_crystal_system      orthorhombic
_space_group_IT_number           31
_space_group_name_Hall           'P 2ac -2'
_space_group_name_H-M_alt        'P m n 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2019-07-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   5.56720(10)
_cell_length_b                   8.2191(2)
_cell_length_c                   4.78410(10)
_cell_measurement_reflns_used    4187
_cell_measurement_temperature    224(8)
_cell_measurement_theta_max      60.1910
_cell_measurement_theta_min      7.9830
_cell_volume                     218.908(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14a (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_environment      N~2~
_diffrn_ambient_temperature      224(8)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.987
_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     89.00 114.00   0.50    0.10    --   72.34 108.00  56.00   50
  2  \w      1.00  78.00   0.50    0.10    --   72.34-108.00 -40.00  154
  3  \w   -117.00 -92.00   0.50    0.10    --  -74.84-108.00 -40.00   50
  4  \w   -102.00 -16.00   0.50    0.10    --  -74.84 108.00  56.00  172
  5  \w    -14.00  11.00   0.50    0.10    --   -1.25 -99.00  30.00   50
  6  \w    -30.00  14.00   0.50    0.10    --   -1.25 -77.00   0.00   88
  7  \w    -14.00  31.00   0.50    0.10    --   -1.25 -99.00 -60.00   90
  8  \w     -6.00  20.00   0.50    0.10    --   -1.25 -99.00  60.00   52
  9  \w    -71.00 -45.00   0.50    0.10    --   -1.25 -77.00   0.00   52
 10  \w     -7.00  28.00   0.50    0.10    --   -1.25 -99.00 150.00   70
 11  \w    -72.00 -25.00   0.50    0.10    --   -1.25 -38.00 -90.00   94
 12  \w      5.00  32.00   0.50    0.10    --   -1.25 -99.00-180.00   54
 13  \w     49.00  97.00   0.50    0.10    --   72.34  77.00 -90.00   96
 14  \w     49.00  84.00   0.50    0.10    --   72.34  77.00 -30.00   70
 15  \w    109.00 135.00   0.50    0.10    --   72.34  77.00 -30.00   52
 16  \w     81.00 141.00   0.50    0.10    --   72.34 125.00-180.00  120
 17  \w     56.00  95.00   0.50    0.10    --   72.34  57.00  60.00   78
 18  \w     50.00  79.00   0.50    0.10    --   72.34  77.00 150.00   58
 19  \w     56.00  84.00   0.50    0.10    --   72.34  57.00  90.00   56
 20  \w      1.00  44.00   0.50    0.10    --   72.34 -99.00-120.00   86
 21  \w     58.00  83.00   0.50    0.10    --   72.34  38.00-120.00   50
 22  \w     53.00  79.00   0.50    0.10    --   72.34 -99.00-120.00   52
 23  \w     59.00  93.00   0.50    0.10    --   72.34  57.00-120.00   68
 24  \w     51.00 143.00   0.50    0.10    --   72.34  77.00  90.00  184
 25  \w   -105.00 -53.00   0.50    0.10    --  -74.84 -77.00   0.00  104
 26  \w    -96.00 -60.00   0.50    0.10    --  -74.84 -38.00  30.00   72
 27  \w    -81.00 -56.00   0.50    0.10    --  -74.84 -77.00-150.00   50
 28  \w   -147.00-100.00   0.50    0.10    --  -74.84-125.00-120.00   94
 29  \w    -85.00 -53.00   0.50    0.10    --  -74.84 -77.00-180.00   64
 30  \w   -137.00-112.00   0.50    0.10    --  -74.84 -77.00-150.00   50
 31  \w   -144.00 -79.00   0.50    0.10    --  -74.84-125.00  30.00  130
 32  \w    -94.00 -51.00   0.50    0.10    --  -74.84 -77.00 120.00   86
 33  \w    -99.00 -53.00   0.50    0.10    --  -74.84 -77.00 150.00   92
 34  \w   -139.00 -53.00   0.50    0.10    --  -74.84 -77.00 -30.00  172
 35  \w   -143.00-117.00   0.50    0.10    --  -74.84 -77.00 120.00   52
 36  \w    -87.00 -53.00   0.50    0.10    --  -74.84 -77.00-120.00   68
 37  \w    -88.00 -59.00   0.50    0.10    --  -74.84 -46.00 143.64   58
 38  \w    -78.00 -51.00   0.50    0.10    --  -74.84 -77.00  60.00   54
 39  \w   -147.00 -99.00   0.50    0.10    --  -74.84 -46.00 143.64   96
 40  \w    -92.00 -63.00   0.50    0.10    --  -74.84 -38.00-120.00   58
 41  \w   -122.00 -60.00   0.50    0.10    --  -74.84 -45.00-129.22  124
 42  \w    -85.00  -1.00   0.50    0.10    --  -74.84  38.00  60.00  168
 43  \w   -134.00-108.00   0.50    0.10    --  -74.84 -77.00  60.00   52
 44  \w    -91.00  -5.00   0.50    0.10    --  -74.84  57.00-120.00  172
 45  \w    -87.00 -52.00   0.50    0.10    --  -74.84 -77.00  30.00   70
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0183893000
_diffrn_orient_matrix_UB_12      -0.1569317000
_diffrn_orient_matrix_UB_13      -0.0721068000
_diffrn_orient_matrix_UB_21      -0.2304032000
_diffrn_orient_matrix_UB_22      -0.0232834000
_diffrn_orient_matrix_UB_23      0.0696801000
_diffrn_orient_matrix_UB_31      -0.0666253000
_diffrn_orient_matrix_UB_32      0.0369929000
_diffrn_orient_matrix_UB_33      -0.2614211000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.0517
_diffrn_reflns_av_unetI/netI     0.0226
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_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       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            4271
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         60.275
_diffrn_reflns_theta_min         4.678
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    9.786
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62651
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.14a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.676
_exptl_crystal_description       prism
_exptl_crystal_F_000             176
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.399
_refine_diff_density_min         -0.314
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details
;
 Flack x determined using 230 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.029(12)
_refine_ls_extinction_coef       0.022(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     50
_refine_ls_number_reflns         535
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0184
_refine_ls_R_factor_gt           0.0183
_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^)+(0.0370P)^2^+0.0200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0459
_refine_ls_wR_factor_ref         0.0460
_reflns_Friedel_coverage         0.760
_reflns_Friedel_fraction_full    0.974
_reflns_Friedel_fraction_max     0.947
_reflns_number_gt                532
_reflns_number_total             535
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm9b03950_si_001.cif
_cod_data_source_block           x
_cod_depositor_comments          'Adding full bibliography for 4003140.cif.'
_cod_database_code               4003140
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'K Mg O P'
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     56.82
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All O(H) groups
;
_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 7.130
_oxdiff_exptl_absorpt_empirical_full_min 0.275