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_4518228
_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 H39.62 O28 Zn2, 7(H2 O)'
_chemical_formula_sum            'C46 H53.62 O35 Zn2'
_chemical_formula_weight         1297.25
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-10-12
_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                 95.6148(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.90641(18)
_cell_length_b                   6.99799(5)
_cell_length_c                   22.92769(14)
_cell_measurement_reflns_used    22129
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      68.7070
_cell_measurement_theta_min      2.7700
_cell_volume                     5094.75(6)
_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_temperature      100.00(10)
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_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  33.00   0.50    3.74    --  -41.49  15.00-174.00  196
  2  \w   -116.00 -18.00   0.50    3.74    --  -41.49 -15.00  15.00  196
  3  \w     18.00 116.00   0.50    3.74    --   41.49  15.00-174.00  196
  4  \w     73.00 158.00   0.50   14.96    --   96.95  15.00-174.00  170
  5  \w     23.00 121.00   0.50   14.96    --   96.95 -15.00  15.00  196
  6  \w    -61.00  23.00   0.50    3.74    --  -41.49  54.00 -60.00  168
  7  \w   -100.00 -10.00   0.50    3.74    --  -41.49 138.00-150.00  180
  8  \w   -110.00 -29.00   0.50    3.74    --  -41.49 -32.00   0.00  162
  9  \w    -64.00  24.00   0.50    3.74    --  -41.49  65.00 150.00  176
 10  \w   -108.00 -15.00   0.50    3.74    --  -41.49 -77.00  30.00  186
 11  \w    -24.00  64.00   0.50    3.74    --   41.49 -65.00 -30.00  176
 12  \w     29.00 110.00   0.50    3.74    --   41.49  32.00 -30.00  162
 13  \w    -33.00  65.00   0.50    3.74    --   41.49 -15.00  15.00  196
 14  \w     23.00 109.00   0.50   14.96    --   96.95 -96.00 -60.00  172
 15  \w     84.00 158.00   0.50   14.96    --   96.95  25.00 -30.00  148
 16  \w     31.00 132.00   0.50   14.96    --   96.95-145.00   0.00  202
 17  \w     81.00 158.00   0.50   14.96    --   96.95  42.00  60.00  154
 18  \w     30.00 117.00   0.50   14.96    --   96.95-117.00  90.00  174
 19  \w     76.00 158.00   0.50   14.96    --   96.95  59.00  30.00  164
 20  \w     32.00 118.00   0.50   14.96    --   96.95 -59.00 -30.00  172
 21  \w     31.00 121.00   0.50   14.96    --   96.95 -68.00 -90.00  180
 22  \w     31.00 132.00   0.50   14.96    --   96.95-145.00  90.00  202
 23  \w     26.00 110.00   0.50   14.96    --   96.95 -25.00 -90.00  168
 24  \w     84.00 158.00   0.50   14.96    --   96.95  33.00-180.00  148
 25  \w     31.00 121.00   0.50   14.96    --   96.95 -68.00  90.00  180
 26  \w   -108.00 -15.00   0.50    3.74    --  -41.49 -77.00   0.00  186
 27  \w   -108.00 -15.00   0.50    3.74    --  -41.49 -77.00  90.00  186
 28  \w   -108.00 -15.00   0.50    3.74    --  -41.49 -77.00 -30.00  186
 29  \w   -108.00 -15.00   0.50    3.74    --  -41.49 -77.00-120.00  186
 30  \w   -108.00 -15.00   0.50    3.74    --  -41.49 -77.00-150.00  186
 31  \w   -107.00 -19.00   0.50    3.74    --  -41.49 -65.00 -90.00  176
 32  \w   -108.00 -15.00   0.50    3.74    --  -41.49 -77.00 150.00  186
 33  \w    -68.00  25.00   0.50    3.74    --  -41.49  77.00-180.00  186
 34  \w     15.00 108.00   0.50    3.74    --   41.49  77.00 -30.00  186
 35  \w     15.00 108.00   0.50    3.74    --   41.49  77.00-180.00  186
 36  \w     15.00 108.00   0.50    3.74    --   41.49  77.00  60.00  186
 37  \w     15.00 108.00   0.50    3.74    --   41.49  77.00 120.00  186
 38  \w     22.00 106.00   0.50    3.74    --   41.49  54.00-120.00  168
 39  \w     73.00 158.00   0.50   14.96    --   96.95  68.00-150.00  170
 40  \w     77.00 158.00   0.50   14.96    --   96.95  50.00   0.00  162
 41  \w     77.00 158.00   0.50   14.96    --   96.95  50.00 -90.00  162
 42  \w     73.00 158.00   0.50   14.96    --   96.95  68.00  90.00  170
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0280
_diffrn_reflns_av_unetI/netI     0.0168
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            31035
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.853
_diffrn_reflns_theta_min         2.783
_exptl_absorpt_coefficient_mu    2.150
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.409
_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            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.691
_exptl_crystal_description       needle
_exptl_crystal_F_000             2678
_exptl_crystal_size_max          0.405
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.024
_refine_diff_density_max         0.430
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         4714
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.230
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0304
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0378P)^2^+10.5473P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0782
_refine_ls_wR_factor_ref         0.0797
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4429
_reflns_number_total             4714
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao0c03320_si_002.cif
_cod_data_source_block           18vlmirr13c
_cod_depositor_comments
'Adding full bibliography for 4518227--4518229.cif.'
_cod_original_cell_volume        5094.75(5)
_cod_database_code               4518228
_shelx_shelxl_version_number     2016/6
_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. Restrained distances
 O12-O12
 0.85 with sigma of 0.02
 O12-H12A = O16-H16A
 0.85 with sigma of 0.02
3. Others
 Fixed Sof: H18A(0.5) H18B(0.5)
4.a Free rotating group:
 O17(H17A,H17B), O16(H16A,H16B), O15(H15A,H15B), O18(H18A,H18B)
4.b Rotating group:
 O13(H13A), O14(H14A,H14B)
4.c Ternary CH refined with riding coordinates:
 C12(H12B)
4.d Secondary CH2 refined with riding coordinates:
 C13(H13B,H13C), C11(H11A,H11B)
4.e Aromatic/amide H refined with riding coordinates:
 C15(H15), C17(H17), C3(H3), C7(H7), C21(H21), C8(H8), C16(H16), C9(H9)
;
_shelx_res_checksum              94527
_shelx_hkl_checksum              17719
_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
;