Rapid Dissolution of BaSO<sub>4</sub> by Macropa, an 18-Membered Macrocycle with High Affinity for Ba<sup>2</sup>.
Thiele, Nikki A.; MacMillan, Samantha N.; Wilson, Justin J.; Journal of the American Chemical Society 140 (2018) 17071–17078; doi:10.1021/jacs.8b08704

data_4133155
_publ_section_title
;
 Rapid Dissolution of BaSO<sub>4</sub> by Macropa, an 18-Membered
 Macrocycle with High Affinity for Ba<sup>2</sup>.
;
_journal_issue                   49
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17071
_journal_page_last               17078
_journal_paper_doi               10.1021/jacs.8b08704
_journal_volume                  140
_journal_year                    2018
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C32 H40 Ba N4 O13 S2, 8(H2 O)'
_chemical_formula_sum            'C32 H56 Ba N4 O21 S2'
_chemical_formula_weight         1034.26
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-10-26
_audit_creation_method
;
Olex2 1.2-ac3
(compiled 2016.08.26 svn.r3337 for Rigaku Oxford Diffraction, GUI svn.r5221)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   28.83060(10)
_cell_length_b                   21.51320(10)
_cell_length_c                   13.92600(10)
_cell_measurement_reflns_used    30901
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      78.3370
_cell_measurement_theta_min      4.0680
_cell_volume                     8637.44(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_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      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_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  \w    -39.00  81.00   0.50    0.62    --    0.00  57.00-120.00  240
  2  \w     91.00 150.00   0.50    2.48    --   62.87 125.00-180.00  118
  3  \w     82.00 178.00   0.50    2.48    --  125.75  50.00-120.00  192
  4  \w    100.00 178.00   0.50    2.48    --  125.75 111.00 -30.00  156
  5  \w    100.00 178.00   0.50    2.48    --  125.75 111.00 120.00  156
  6  \w     91.00 150.00   0.50    2.48    --   62.87 125.00  60.00  118
  7  \w     91.00 150.00   0.50    2.48    --   62.87 125.00 120.00  118
  8  \w     87.00 178.00   0.50    2.48    --  125.75  63.00 120.00  182
  9  \w     87.00 178.00   0.50    2.48    --  125.75  63.00  90.00  182
 10  \w     87.00 178.00   0.50    2.48    --  125.75  63.00 -90.00  182
 11  \w     82.00 178.00   0.50    2.48    --  125.75  50.00  60.00  192
 12  \w     80.00 178.00   0.50    2.48    --  125.75  77.00 -30.00  196
 13  \w     80.00 178.00   0.50    2.48    --  125.75  77.00 -60.00  196
 14  \w     80.00 178.00   0.50    2.48    --  125.75  77.00-180.00  196
 15  \w     82.00 178.00   0.50    2.48    --  125.75  50.00 -90.00  192
 16  \w     80.00 178.00   0.50    2.48    --  125.75  77.00  90.00  196
 17  \w     60.00 149.00   0.50    2.48    --  125.75 178.00  60.00  178
 18  \w     60.00 149.00   0.50    2.48    --  125.75 178.00 -30.00  178
 19  \w     60.00 149.00   0.50    2.48    --  125.75 178.00-180.00  178
 20  \w     60.00 149.00   0.50    2.48    --  125.75 178.00-150.00  178
 21  \w     62.00 178.00   0.50    2.48    --  125.75  37.00-150.00  232
 22  \w     31.00 121.00   0.50    2.48    --   62.87-125.00 -90.00  180
 23  \w     43.00 165.00   0.50    2.48    --  125.75 -63.00 -90.00  244
 24  \w     34.00 172.00   0.50    2.48    --  125.75 -77.00-120.00  276
 25  \w     43.00 165.00   0.50    2.48    --  125.75 -63.00-150.00  244
 26  \w     36.00 115.00   0.50    2.48    --  125.75-111.00 -90.00  158
 27  \w     34.00 172.00   0.50    2.48    --  125.75 -77.00  30.00  276
 28  \w     43.00 165.00   0.50    2.48    --  125.75 -63.00  30.00  244
 29  \w     35.00 178.00   0.50    2.48    --  125.75  25.00  90.00  286
 30  \w     60.00 149.00   0.50    2.48    --  125.75 178.00 150.00  178
 31  \w     35.00 178.00   0.50    2.48    --  125.75  25.00  30.00  286
 32  \w     32.00 178.00   0.50    2.48    --  125.75 -91.00-120.00  292
 33  \w     36.00 115.00   0.50    2.48    --  125.75-111.00-150.00  158
 34  \w     36.00 115.00   0.50    2.48    --  125.75-111.00 -30.00  158
 35  \w     36.00 115.00   0.50    2.48    --  125.75-111.00  90.00  158
 36  \w     32.00 178.00   0.50    2.48    --  125.75 -91.00 -30.00  292
 37  \w     36.00 115.00   0.50    2.48    --  125.75-111.00-180.00  158
 38  \w     36.00 115.00   0.50    2.48    --  125.75-111.00  30.00  158
 39  \w     36.00 115.00   0.50    2.48    --  125.75-111.00 150.00  158
 40  \w     34.00 172.00   0.50    2.48    --  125.75 -77.00 150.00  276
 41  \w     30.00 178.00   0.50    2.48    --  125.75 -12.00 120.00  296
 42  \w     32.00 178.00   0.50    2.48    --  125.75 -91.00  90.00  292
 43  \w      9.00  37.00   0.50    2.48    --   62.87  94.00-156.30   56
 44  \w      9.00  37.00   0.50    2.48    --   62.87  94.00 -85.10   56
 45  \w     11.00  45.00   0.50    2.48    --   62.87  91.00 -26.31   68
 46  \w      9.00  37.00   0.50    2.48    --   62.87  94.00  52.57   56
 47  \w      9.00  37.00   0.50    2.48    --   62.87  94.00 133.89   56
 48  \w    -94.00 -10.00   0.50    2.48    --  -62.87 125.00  60.00  168
 49  \w    -89.00 -16.00   0.50    2.48    -- -104.25 111.00  60.00  146
 50  \w   -109.00  26.00   0.50    2.48    --  -62.87  77.00  60.00  270
 51  \w    -39.00  81.00   0.50    0.62    --    0.00  57.00-180.00  240
 52  \w     -4.00  57.00   0.50    0.62    --    0.00 -99.00-180.00  122
 53  \w     -4.00  57.00   0.50    0.62    --    0.00 -99.00  30.00  122
 54  \w   -100.00 -38.00   0.50    0.62    --    0.00-178.00-180.00  124
 55  \w   -100.00 -38.00   0.50    0.62    --    0.00-178.00 -60.00  124
 56  \w   -158.00  26.00   0.50    2.48    --  -62.87 -15.00 150.00  368
 57  \w   -114.00  23.00   0.50    2.48    --  -62.87  45.00 -60.00  274
 58  \w    -98.00 -36.00   0.50    0.62    --    0.00 178.00  90.00  124
 59  \w    -98.00 -36.00   0.50    0.62    --    0.00 178.00 150.00  124
 60  \w   -177.00 -62.00   0.50    2.48    -- -104.25 -53.00-133.78  230
 61  \w   -156.00 -80.00   0.50    2.48    --  -62.87 -94.00   0.00  152
 62  \w   -148.00 -14.00   0.50    2.48    --  -62.87 -45.00  30.00  268
 63  \w   -177.00 -78.00   0.50    2.48    -- -104.25-111.00-180.00  198
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0375827000
_diffrn_orient_matrix_UB_12      -0.0431894000
_diffrn_orient_matrix_UB_13      -0.0416187000
_diffrn_orient_matrix_UB_21      -0.0361594000
_diffrn_orient_matrix_UB_22      0.0522939000
_diffrn_orient_matrix_UB_23      0.0104741000
_diffrn_orient_matrix_UB_31      0.0116408000
_diffrn_orient_matrix_UB_32      0.0229834000
_diffrn_orient_matrix_UB_33      -0.1019551000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_av_unetI/netI     0.0120
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            40654
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.015
_diffrn_reflns_theta_min         4.081
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.792
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.543
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
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    1.591
_exptl_crystal_description       needle
_exptl_crystal_F_000             4256
_exptl_crystal_size_max          0.142
_exptl_crystal_size_mid          0.035
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.320
_refine_diff_density_min         -0.239
_refine_diff_density_rms         0.041
_refine_ls_abs_structure_details
;
 Flack x determined using 1795 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.0120(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         3955
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0144
_refine_ls_R_factor_gt           0.0142
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0239P)^2^+6.9937P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0374
_refine_ls_wR_factor_ref         0.0375
_reflns_Friedel_coverage         0.846
_reflns_Friedel_fraction_full    0.926
_reflns_Friedel_fraction_max     0.924
_reflns_number_gt                3927
_reflns_number_total             3955
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b08704_si_002.cif
_cod_data_source_block           Ba-macroquin-SO3
_cod_database_code               4133155
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         BaC32H56N4O21S2
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O3_$2-H3_$2 = O9_$6-H9A_$6 = O9_$6-H9B_$6 = O10_$2-H10A_$2 = O10_$2-H10B_$2 =
 O8-H8B = O8-H8A = O11_$7-H11B_$7 = O11_$7-H11A_$7
 0.84 with sigma of 0.02
 O7-H7
 0.84 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B)
3.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C13(H13), C14(H14)
;
_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 1.431
_oxdiff_exptl_absorpt_empirical_full_min 0.769