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_7713414
_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         'C4 H4 Mg2 O14 P2, H2 O, C7 H20 N2'
_chemical_formula_sum            'C11 H26 Mg2 N2 O15 P2'
_chemical_formula_weight         536.90
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 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                110.668(6)
_cell_angle_beta                 104.445(6)
_cell_angle_gamma                107.384(6)
_cell_formula_units_Z            1
_cell_length_a                   8.2680(6)
_cell_length_b                   8.8920(6)
_cell_length_c                   9.5432(6)
_cell_measurement_reflns_used    2566
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4960
_cell_measurement_theta_min      4.0070
_cell_volume                     574.86(9)
_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_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9595
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega   -1.00   83.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       15.7256   57.0000  -60.0000 84

  2 omega  -20.00   55.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       15.7256  -99.0000   90.0000 75

  3 omega  -20.00   55.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       15.7256  -99.0000 -180.0000 75

  4 omega  -11.00   83.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       15.7256   77.0000   30.0000 94

  5 omega   35.00   88.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       15.7256  178.0000 -180.0000 53

  6 omega  -54.00   85.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       15.7256    0.0000  -90.0000 139

  7 omega  -52.00   20.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       15.7256  -57.0000 -120.0000 72
;
_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      0.0187346000
_diffrn_orient_matrix_UB_12      0.0866146000
_diffrn_orient_matrix_UB_13      0.0082675000
_diffrn_orient_matrix_UB_21      -0.0929818000
_diffrn_orient_matrix_UB_22      -0.0161065000
_diffrn_orient_matrix_UB_23      -0.0120955000
_diffrn_orient_matrix_UB_31      0.0245127000
_diffrn_orient_matrix_UB_32      0.0335734000
_diffrn_orient_matrix_UB_33      0.0853211000
_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  0.0297
_diffrn_reflns_av_unetI/netI     0.0529
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            7053
_diffrn_reflns_point_group_measured_fraction_full 0.946
_diffrn_reflns_point_group_measured_fraction_max 0.933
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         3.777
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.317
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90918
_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    1.551
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             280
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.214
_refine_diff_density_min         -0.252
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details
;
 Flack x determined using 1720 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.04(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4394
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0397
_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^)+(0.0279P)^2^+0.0476P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0750
_refine_ls_wR_factor_ref         0.0791
_reflns_Friedel_coverage         0.871
_reflns_Friedel_fraction_full    0.895
_reflns_Friedel_fraction_max     0.868
_reflns_number_gt                4072
_reflns_number_total             4394
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01885g2.cif
_cod_data_source_block           2
_cod_original_cell_volume        574.86(7)
_cod_database_code               7713414
_shelxl_version_number           2014-1
_shelx_estimated_absorpt_t_max   0.917
_shelx_estimated_absorpt_t_min   0.895
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups, All P(H) groups
2.a Riding coordinates:
 P1(H1A), P2(H2A)
2.b Free rotating group:
 OW1(HW1A,HW1B)
2.c Ternary CH refined with riding coordinates:
 N1(H1), N2(H2)
2.d Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B)
2.e Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C)
2.f Idealised tetrahedral OH refined as rotating group:
 O3(H3), O6(H6)
;
_olex2_submission_special_instructions 'No special instructions were received'