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_4518227
_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         'C46 H46 Ca2 O32, 4(H2 O)'
_chemical_formula_sum            'C46 H54 Ca2 O36'
_chemical_formula_weight         1263.05
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-10-14
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 99.495(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.0293(3)
_cell_length_b                   29.2917(7)
_cell_length_c                   12.7862(4)
_cell_measurement_reflns_used    7344
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      68.1520
_cell_measurement_theta_min      3.0170
_cell_volume                     2596.61(15)
_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    -65.00  24.00   0.50    4.31    --  -41.24  68.00 -24.00  178
  2  \w   -107.00 -18.00   0.50    4.31    --  -41.24 -68.00-157.00  178
  3  \w     31.00 121.00   0.50   17.26    --   96.95 -68.00-157.00  180
  4  \w     73.00 158.00   0.50   17.26    --   96.95  68.00 -24.00  170
  5  \w    -53.00  27.00   0.50    4.31    --  -41.24  32.00 120.00  160
  6  \w    -99.00 -10.00   0.50    4.31    --  -41.24 138.00  60.00  178
  7  \w    -17.00  79.00   0.50    4.31    --   41.24-104.00  60.00  192
  8  \w    -27.00  53.00   0.50    4.31    --   41.24 -32.00 -60.00  160
  9  \w     29.00 109.00   0.50    4.31    --   41.24  32.00 -60.00  160
 10  \w     29.00 109.00   0.50    4.31    --   41.24  32.00 120.00  160
 11  \w     18.00 107.00   0.50    4.31    --   41.24  68.00 -24.00  178
 12  \w    -24.00  65.00   0.50    4.31    --   41.24 -68.00-157.00  178
 13  \w     70.00 158.00   0.50   17.26    --   96.95  77.00 -90.00  176
 14  \w     76.00 158.00   0.50   17.26    --   96.95  59.00 -60.00  164
 15  \w     77.00 158.00   0.50   17.26    --   96.95 117.00   0.00  162
 16  \w     80.00 158.00   0.50   17.26    --   96.95  96.00-150.00  156
 17  \w     30.00 113.00   0.50   17.26    --   96.95-117.00-150.00  166
 18  \w     32.00 113.00   0.50   17.26    --   96.95 -42.00  90.00  162
 19  \w     29.00 109.00   0.50   17.26    --   96.95 -33.00-150.00  160
 20  \w     26.00 110.00   0.50   17.26    --   96.95 -25.00   0.00  168
 21  \w     32.00 117.00   0.50   17.26    --   96.95 -50.00   0.00  170
 22  \w     76.00 158.00   0.50   17.26    --   96.95  59.00-120.00  164
 23  \w     81.00 158.00   0.50   17.26    --   96.95  42.00 -30.00  154
 24  \w     80.00 158.00   0.50   17.26    --   96.95  96.00-120.00  156
 25  \w     18.00 107.00   0.50    4.31    --   41.24  65.00 150.00  178
 26  \w     15.00  84.00   0.50    4.31    --   41.24  77.00  60.00  138
 27  \w     18.00 107.00   0.50    4.31    --   41.24  65.00  30.00  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      -0.0168967000
_diffrn_orient_matrix_UB_12      0.0004831000
_diffrn_orient_matrix_UB_13      0.1185842000
_diffrn_orient_matrix_UB_21      0.1397706000
_diffrn_orient_matrix_UB_22      0.0408090000
_diffrn_orient_matrix_UB_23      0.0176836000
_diffrn_orient_matrix_UB_31      -0.1718898000
_diffrn_orient_matrix_UB_32      0.0331891000
_diffrn_orient_matrix_UB_33      -0.0233914000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_unetI/netI     0.0294
_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       35
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            20731
_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         68.960
_diffrn_reflns_theta_min         3.017
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.905
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78209
_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    1.615
_exptl_crystal_description       plate
_exptl_crystal_F_000             1316
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.657
_refine_diff_density_min         -0.544
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         4797
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0872
_refine_ls_R_factor_gt           0.0791
_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^)+(0.0837P)^2^+7.6456P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1913
_refine_ls_wR_factor_ref         0.1969
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4282
_reflns_number_total             4797
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao0c03320_si_001.cif
_cod_data_source_block           19vlmirr002
_cod_depositor_comments
'Adding full bibliography for 4518227--4518229.cif.'
_cod_database_code               4518227
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C23H16O17N2Ca
_shelx_estimated_absorpt_t_max   0.972
_shelx_estimated_absorpt_t_min   0.760
_reflns_odcompleteness_completeness 99.94
_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, All O(H,H) groups
2.a Free rotating group:
 O18(H18A,H18B), O17(H17A,H17B)
2.b Rotating group:
 O13(H13A,H13B), O14(H14A,H14B), O15(H15A,H15B), O16(H16A,H16B)
2.c Ternary CH refined with riding coordinates:
 C12(H12A)
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              33266
_shelx_hkl_checksum              45467
_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 1.662
_oxdiff_exptl_absorpt_empirical_full_min 0.803