The crystal structure, morphology and mechanical properties of diaquabis(omeprazolate)magnesium dihydrate
Abouhakim, Hanane; Nilsson Lill, Sten O.; Quayle, Michael J.; Norberg, Stefan T.; Hassanpour, Ali; Pask, Christopher M.; Acta Crystallographica Section B 76 (2020) –; doi:10.1107/S2052520620001249

data_2108595
_publ_section_title
;
 The crystal structure, morphology and mechanical properties of
 diaquabis(omeprazolate)magnesium dihydrate
;
_journal_coeditor_code           RM5029
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2052520620001249
_journal_volume                  76
_journal_year                    2020
_chemical_formula_moiety         'C34 H40 Mg N6 O8 S2 , 2H2 O'
_chemical_formula_sum            'C34 H44 Mg N6 O10 S2'
_chemical_formula_weight         785.18
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-02-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 109.91(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.475(9)
_cell_length_b                   8.051(2)
_cell_length_c                   14.190(5)
_cell_measurement_reflns_used    455
_cell_measurement_temperature    120.0(2)
_cell_measurement_theta_max      68.5000
_cell_measurement_theta_min      6.2060
_cell_volume                     1877.1(14)
_computing_cell_refinement       'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.43c (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      120.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.940
_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    -63.00 -19.00   1.00   45.00    --  -40.79  57.00  90.00   44
  2  \w    -61.00 -18.00   1.00   45.00    --  -40.79  48.00 -81.00   43
  3  \w     19.00  80.00   1.00   45.00    --   40.79  64.00  85.84   61
  4  \w     11.00 100.00   1.00   45.00    --   40.79  64.00 149.97   89
  5  \w     40.00  69.00   1.00   45.00    --   40.79 -65.00 101.61   29
  6  \w     21.00  46.00   1.00   45.00    --   40.79  64.00-117.38   25
  7  \w     63.00 112.00   1.00  200.00    --  106.02 -65.00-171.34   49
  8  \w     78.00 177.00   1.00  200.00    --  106.02  30.00-180.00   99
  9  \w     31.00 119.00   1.00  200.00    --  106.02 -30.00   0.00   88
 10  \w     35.00 100.00   1.00  200.00    --  106.02 -65.00  34.43   65
 11  \w     57.00 103.00   1.00  200.00    --  106.02 -65.00 142.31   46
 12  \w    145.00 172.00   1.00  200.00    --  106.02  45.00-120.00   27
 13  \w     64.00  91.00   1.00  200.00    --  106.02 -65.00 -77.03   27
 14  \w     95.00 123.00   1.00  200.00    --  106.02 -45.00  90.00   28
 15  \w     66.00 100.00   1.00  200.00    --  106.02 -65.00 -47.12   34
 16  \w     45.00  89.00   1.00  200.00    --  106.02 -65.00   1.02   44
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0510322000
_diffrn_orient_matrix_UB_12      -0.0773748000
_diffrn_orient_matrix_UB_13      -0.0584390000
_diffrn_orient_matrix_UB_21      0.0227665000
_diffrn_orient_matrix_UB_22      0.1751027000
_diffrn_orient_matrix_UB_23      -0.0255674000
_diffrn_orient_matrix_UB_31      0.0753539000
_diffrn_orient_matrix_UB_32      -0.0007697000
_diffrn_orient_matrix_UB_33      0.0960500000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1656
_diffrn_reflns_av_unetI/netI     0.2009
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.940
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8269
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.575
_diffrn_reflns_theta_min         5.384
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.994
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.812
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.43c (Rigaku Oxford Diffraction, 2018)
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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_description       plate
_exptl_crystal_F_000             828
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.713
_refine_diff_density_min         -0.660
_refine_diff_density_rms         0.195
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         3546
_refine_ls_number_restraints     216
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.2299
_refine_ls_R_factor_gt           0.1496
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3519
_refine_ls_wR_factor_ref         0.4164
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1689
_reflns_number_total             3546
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            rm5029sup1.cif
_cod_data_source_block           I
_cod_database_code               2108595
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C68  H88  Mg2  N12  O20  S4'
_shelx_estimated_absorpt_t_max   0.980
_shelx_estimated_absorpt_t_min   0.810
_reflns_odcompleteness_completeness 95.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Rigid body (RIGU) restrains
 S1, Mg1, O1, O2, O3, O4, N1, N2, N3, C1, C2, C3, C4, C5, C6, C7, C8, C9, C10,
 C11, C12, C13, C14, C15, C16, C17
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Free rotating group:
 O5(H5A,H5B)
3.b Rotating group:
 O4(H4A,H4B)
3.c Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B)
3.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C14(H14)
3.e Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C)
;
_olex2_date_sample_data_collection 2018-11-26
_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 2.098
_oxdiff_exptl_absorpt_empirical_full_min 0.579
_cod_database_fobs_code 2108595