Solvent-free synthesis of magnesium phosphite-oxalates showing second-harmonic generation responses
Luo, Lisiteng; Wen, Xuemei; Cheng, Juan; Li, Jing; Zeng, Hongmei; Zou, Guohong; Lin, Zhien; Dalton Transactions  (2023) –; doi:10.1039/D3DT01885G

data_7713413
_publ_section_title
;
 Solvent-free synthesis of magnesium phosphite-oxalates showing
 second-harmonic generation responses
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01885G
_journal_year                    2023
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C2 H4 Mg O10 P2, C2 H10 N2'
_chemical_formula_sum            'C4 H14 Mg N2 O10 P2'
_chemical_formula_weight         336.42
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-06-07
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-06-16 deposited with the CCDC.	2023-07-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.714(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.3313(2)
_cell_length_b                   9.0913(2)
_cell_length_c                   8.7803(2)
_cell_measurement_reflns_used    4068
_cell_measurement_temperature    292.9(2)
_cell_measurement_theta_max      72.6690
_cell_measurement_theta_min      5.0430
_cell_volume                     583.99(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      292.9(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9595
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -33.00  106.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5421    0.0000  -30.0000 139

  2 omega   10.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5421   77.0000  -60.0000 94

  3 omega  -31.00   53.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -57.0000 -120.0000 84

  4 omega   23.00   90.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5421 -125.0000   90.0000 67

  5 omega   40.00   98.00   1.0000    2.7600
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000   30.0000 58

  6 omega   87.00  178.00   1.0000    2.7600
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000   60.0000 91

  7 omega   91.00  176.00   1.0000    2.7600
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000  150.0000 85

  8 omega   38.00   91.00   1.0000    2.7600
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  -30.0000 53

  9 omega   38.00   91.00   1.0000    2.7600
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  150.0000 53

 10 omega   38.00   91.00   1.0000    2.7600
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   30.0000 53

 11 omega   39.00  109.00   1.0000    2.7600
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000 -180.0000 70

 12 omega   39.00  109.00   1.0000    2.7600
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000  -90.0000 70

 13 omega   40.00   98.00   1.0000    2.7600
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000 -120.0000 58

 14 omega   20.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5421   57.0000  150.0000 84

 15 omega   10.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5421   77.0000 -150.0000 94

 16 omega   20.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5421   57.0000   60.0000 84

 17 omega  -31.00   53.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -57.0000  150.0000 84

 18 omega   81.00  176.00   1.0000    2.7600
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -120.0000 95

 19 omega   87.00  178.00   1.0000    2.7600
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000 -120.0000 91

 20 omega   39.00  109.00   1.0000    2.7600
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000   30.0000 70

 21 omega   91.00  176.00   1.0000    2.7600
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000    0.0000 85

 22 omega   87.00  178.00   1.0000    2.7600
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000  -30.0000 91

 23 omega   91.00  176.00   1.0000    2.7600
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000 -180.0000 85

 24 omega   81.00  176.00   1.0000    2.7600
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -90.0000 95

 25 omega   87.00  178.00   1.0000    2.7600
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000  120.0000 91
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Gemini, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.1245716000
_diffrn_orient_matrix_UB_12      -0.0635014000
_diffrn_orient_matrix_UB_13      -0.1320147000
_diffrn_orient_matrix_UB_21      -0.1182576000
_diffrn_orient_matrix_UB_22      -0.0751973000
_diffrn_orient_matrix_UB_23      0.1161234000
_diffrn_orient_matrix_UB_31      -0.1217777000
_diffrn_orient_matrix_UB_32      0.1379541000
_diffrn_orient_matrix_UB_33      0.0025215000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            5584
_diffrn_reflns_point_group_measured_fraction_full 0.936
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.051
_diffrn_reflns_theta_min         7.019
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.495
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78061
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.913
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             348
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.706
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.110
_refine_ls_abs_structure_details
;
 Flack x determined using 822 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.016(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         1969
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0452
_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^)+(0.0941P)^2^+0.0463P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1168
_refine_ls_wR_factor_ref         0.1184
_reflns_Friedel_coverage         0.772
_reflns_Friedel_fraction_full    0.876
_reflns_Friedel_fraction_max     0.885
_reflns_number_gt                1932
_reflns_number_total             1969
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01885g2.cif
_cod_data_source_block           1
_cod_database_code               7713413
_shelxl_version_number           2014-1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All N(H,H,H) groups, All O(H) groups, All P(H) groups
2.a Riding coordinates:
 P1(H1), P2(H2)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B)
2.c Me refined with riding coordinates:
 N1(H1A,H1B,H1C), N2(H2A,H2B,H2C)
2.d Tetrahedral OH refined with riding coordinates:
 O3(H3), O6(H6)
;
_olex2_submission_special_instructions 'No special instructions were received'