New Data on Crystal Phases in the System MgSO4–OC(NH2)2–H2O
Nikolova, Rositsa; Kostov-Kytin, Vladislav; Petrova, Nadia; Kossev, Krasimir; Titorenkova, Rositsa; Velyanova, Gergana; Crystals 14 (2024) 227–; doi:10.3390/cryst14030227

data_1571115
_publ_section_title
;
 New Data on Crystal Phases in the System MgSO4--OC(NH2)2--H2O
;
_journal_issue                   3
_journal_name_full               Crystals
_journal_page_first              227
_journal_paper_doi               10.3390/cryst14030227
_journal_volume                  14
_journal_year                    2024
_chemical_formula_moiety         'C H8 Mg N2 O7 S'
_chemical_formula_sum            'C H8 Mg N2 O7 S'
_chemical_formula_weight         216.46
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_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             2024-02-19
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_cell_angle_alpha                68.758(13)
_cell_angle_beta                 77.177(13)
_cell_angle_gamma                71.498(12)
_cell_formula_units_Z            2
_cell_length_a                   5.2140(8)
_cell_length_b                   7.7014(9)
_cell_length_c                   10.4275(16)
_cell_measurement_reflns_used    3637
_cell_measurement_temperature    290(2)
_cell_measurement_theta_max      36.7260
_cell_measurement_theta_min      2.0870
_cell_volume                     367.38(10)
_computing_cell_refinement       'CrysAlisPro 1.171.42.58a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.58a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.58a (Rigaku OD, 2022)'
_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    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      290(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \f     -9.39 350.61   2.00   24.70  79.47  -6.39  28.85    --   180
  2  \w    -65.46  -1.46   2.00   24.70    --  -22.79  94.56   1.16   32
  3  \w    -65.46  -1.46   2.00   24.70    --  -22.79  94.56 145.16   32
  4  \w    -92.18  13.82   2.00   24.70    --   -6.39 -59.25 -51.92   53
  5  \f   -350.61   9.27   2.00   24.70   3.49  -6.39 -28.85    --   180
  6  \w    -45.86   0.14   2.00   24.70    --   -3.19  94.56 -34.84   23
  7  \w    -65.46  -1.46   2.00   24.70    --  -22.79  94.56  73.16   32
  8  \w    -92.18  13.82   2.00   24.70    --   -6.39 -59.25-123.92   53
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0860432000
_diffrn_orient_matrix_UB_12      -0.0605629000
_diffrn_orient_matrix_UB_13      -0.0385786000
_diffrn_orient_matrix_UB_21      -0.1158141000
_diffrn_orient_matrix_UB_22      -0.0178844000
_diffrn_orient_matrix_UB_23      -0.0128081000
_diffrn_orient_matrix_UB_31      -0.0089613000
_diffrn_orient_matrix_UB_32      0.0805970000
_diffrn_orient_matrix_UB_33      -0.0612728000
_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  0.0564
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10667
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.345
_diffrn_reflns_theta_min         2.111
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.534
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87345
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.58a (Rigaku Oxford Diffraction, 2022)
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    1.957
_exptl_crystal_description       block
_exptl_crystal_F_000             224
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.870
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.239
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     112
_refine_ls_number_reflns         1347
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.239
_refine_ls_R_factor_all          0.0762
_refine_ls_R_factor_gt           0.0673
_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^)+(0.0356P)^2^+1.9926P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1474
_refine_ls_wR_factor_ref         0.1511
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1218
_reflns_number_total             1347
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            MgSO4_U_2H2O.cif
_cod_data_source_block           shelx
_cod_database_code               1571115
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups, All O(H,H) groups
2.a Riding coordinates:
 O6(H6a,H6b), O7(H7a,H7b)
2.b X=CH2 refined with riding coordinates:
 N1(H1a,H1b), N2(H2a,H2b)
;
_shelx_res_checksum              23933
_shelx_hkl_checksum              39702
_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 1.575
_oxdiff_exptl_absorpt_empirical_full_min 0.721