Design of Potential Pharmaceutical-Based Metal Complexes Derived from Cromolyn a Mast Cell Stabilizer
Rodríguez, Israel; Flores Bello, Jeaninna; Marie Serrano Valcárcel, Joyce; López-Mejías, Vilmalí; ACS Omega 5 (2020) 29714–29721; doi:10.1021/acsomega.0c03320

data_4518229
_publ_section_title
;
 Design of Potential Pharmaceutical-Based Metal Complexes Derived from
 Cromolyn a Mast Cell Stabilizer
;
_journal_issue                   46
_journal_name_full               'ACS Omega'
_journal_page_first              29714
_journal_page_last               29721
_journal_paper_doi               10.1021/acsomega.0c03320
_journal_volume                  5
_journal_year                    2020
_chemical_formula_moiety         'C23 H24 Mg O16, H2 O'
_chemical_formula_sum            'C23 H26 Mg O17'
_chemical_formula_weight         598.75
_chemical_name_systematic        'Cromolyn-Mg metal complex'
_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
_audit_creation_date             2020-07-03
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-07-03 deposited with the CCDC.	2020-10-19 downloaded from the CCDC.
;
_cell_angle_alpha                100.8990(10)
_cell_angle_beta                 98.9160(10)
_cell_angle_gamma                93.5560(10)
_cell_formula_units_Z            2
_cell_length_a                   7.34210(10)
_cell_length_b                   10.37410(10)
_cell_length_c                   16.8517(2)
_cell_measurement_reflns_used    11636
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      68.6270
_cell_measurement_theta_min      2.6990
_cell_volume                     1239.64(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_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   -108.00 -15.00   0.50    0.50    --  -41.24 -77.00 -80.00  186
  2  \w    -68.00  25.00   0.50    0.50    --  -41.24  77.00  46.00  186
  3  \w     70.00 158.00   0.50    0.50    --   96.95  77.00  46.00  176
  4  \w     30.00 123.00   0.50    0.50    --   96.95 -77.00 -80.00  186
  5  \w    -68.00  25.00   0.50    0.50    --  -41.24  77.00 120.00  186
  6  \w   -113.00 -25.00   0.50    0.50    --  -41.24 -21.00 120.00  176
  7  \w   -108.00 -15.00   0.50    0.50    --  -41.24 -77.00-180.00  186
  8  \w    -79.00  17.00   0.50    0.50    --  -41.24 104.00 150.00  192
  9  \w   -109.00 -29.00   0.50    0.50    --  -41.24 -32.00-180.00  160
 10  \w     15.00 108.00   0.50    0.50    --   41.24  77.00  46.00  186
 11  \w    -31.00  58.00   0.50    0.50    --   41.24 -21.00-120.00  178
 12  \w    -27.00  53.00   0.50    0.50    --   41.24 -32.00  30.00  160
 13  \w    -25.00  68.00   0.50    0.50    --   41.24 -77.00 -80.00  186
 14  \w    -17.00  79.00   0.50    0.50    --   41.24-104.00-150.00  192
 15  \w     75.00 158.00   0.50    0.50    --   96.95  17.00-180.00  166
 16  \w     28.00 127.00   0.50    0.50    --   96.95 -87.00-180.00  198
 17  \w     77.00 158.00   0.50    0.50    --   96.95 117.00 -30.00  162
 18  \w     23.00 109.00   0.50    0.50    --   96.95 -96.00 -30.00  172
 19  \w     29.00 109.00   0.50    0.50    --   96.95 -33.00 -90.00  160
 20  \w     61.00 158.00   0.50    0.50    --   96.95 145.00 -90.00  194
 21  \w     31.00 132.00   0.50    0.50    --   96.95-145.00-120.00  202
 22  \w     80.00 158.00   0.50    0.50    --   96.95  96.00-180.00  156
 23  \w     31.00 132.00   0.50    0.50    --   96.95-145.00-180.00  202
 24  \w     77.00 158.00   0.50    0.50    --   96.95  50.00 150.00  162
 25  \w     76.00 158.00   0.50    0.50    --   96.95  59.00-120.00  164
 26  \w     80.00 158.00   0.50    0.50    --   96.95  96.00  60.00  156
 27  \w     30.00 113.00   0.50    0.50    --   96.95-117.00 -60.00  166
 28  \w     30.00 113.00   0.50    0.50    --   96.95-117.00 -90.00  166
 29  \w     77.00 158.00   0.50    0.50    --   96.95 117.00   0.00  162
 30  \w     30.00 123.00   0.50    0.50    --   96.95 -77.00  30.00  186
 31  \w     84.00 158.00   0.50    0.50    --   96.95  33.00 -30.00  148
 32  \w     29.00 109.00   0.50    0.50    --   96.95 -33.00 150.00  160
 33  \w     30.00 113.00   0.50    0.50    --   96.95-117.00  60.00  166
 34  \w     31.00 121.00   0.50    0.50    --   96.95 -68.00 -30.00  180
 35  \w     32.00 113.00   0.50    0.50    --   96.95 -42.00  60.00  162
 36  \w     73.00 158.00   0.50    0.50    --   96.95  68.00  90.00  170
 37  \w   -108.00 -15.00   0.50    0.50    --  -41.24 -77.00  30.00  186
 38  \w   -108.00 -15.00   0.50    0.50    --  -41.24 -77.00   0.00  186
 39  \w   -108.00 -15.00   0.50    0.50    --  -41.24 -77.00  90.00  186
 40  \w    -58.00  31.00   0.50    0.50    --  -41.24  21.00-150.00  178
 41  \w   -108.00 -15.00   0.50    0.50    --  -41.24 -77.00  60.00  186
 42  \w   -107.00 -18.00   0.50    0.50    --  -41.24 -65.00-150.00  178
 43  \w   -107.00 -18.00   0.50    0.50    --  -41.24 -65.00 120.00  178
 44  \w   -108.00 -15.00   0.50    0.50    --  -41.24 -77.00 -60.00  186
 45  \w     15.00 108.00   0.50    0.50    --   41.24  77.00-150.00  186
 46  \w     15.00 108.00   0.50    0.50    --   41.24  77.00 -90.00  186
 47  \w    -27.00  53.00   0.50    0.50    --   41.24 -32.00-150.00  160
 48  \w     15.00 108.00   0.50    0.50    --   41.24  77.00 -60.00  186
 49  \w     18.00 107.00   0.50    0.50    --   41.24  65.00   0.00  178
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1016523000
_diffrn_orient_matrix_UB_12      0.0457113000
_diffrn_orient_matrix_UB_13      -0.0753801000
_diffrn_orient_matrix_UB_21      -0.1875331000
_diffrn_orient_matrix_UB_22      -0.0384935000
_diffrn_orient_matrix_UB_23      0.0235253000
_diffrn_orient_matrix_UB_31      0.0034295000
_diffrn_orient_matrix_UB_32      0.1396549000
_diffrn_orient_matrix_UB_33      0.0518646000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_av_unetI/netI     0.0213
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19570
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.847
_diffrn_reflns_theta_min         2.710
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.430
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87138
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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    1.604
_exptl_crystal_description       block
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.460
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         4543
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0455
_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^)+(0.0663P)^2^+1.3858P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1224
_refine_ls_wR_factor_ref         0.1246
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4196
_reflns_number_total             4543
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao0c03320_si_003.cif
_cod_data_source_block           19vlmirr001
_cod_depositor_comments
'Adding full bibliography for 4518227--4518229.cif.'
_cod_database_code               4518229
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C23H16O17N2Mg2
_shelx_estimated_absorpt_t_max   0.986
_shelx_estimated_absorpt_t_min   0.804
_reflns_odcompleteness_completeness 99.98
_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 O(H) groups
2.a Free rotating group:
 O17(H17A)
2.b Rotating group:
 O12(H12A)
2.c Ternary CH refined with riding coordinates:
 C12(H12)
2.d Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C13(H13C,H13D)
2.e Aromatic/amide H refined with riding coordinates:
 C3(H3), C7(H7), C8(H8), C9(H9), C15(H15), C16(H16), C17(H17), C21(H21)
2.f Idealised tetrahedral OH refined as rotating group:
 O6(H6)
;
_shelx_res_checksum              26379
_shelx_hkl_checksum              7995
_olex2_exptl_crystal_mounting_method 'in paratone oil. '
_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 1.223
_oxdiff_exptl_absorpt_empirical_full_min 0.825