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_4133153
_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         'C29 H42 Ba N5 O9, Cl O4, C4 H10 O'
_chemical_formula_sum            'C33 H52 Ba Cl N5 O14'
_chemical_formula_weight         915.58
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-07-18
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5335)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.3442(6)
_cell_length_b                   13.0303(5)
_cell_length_c                   21.5769(9)
_cell_measurement_reflns_used    9946
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      25.320
_cell_measurement_theta_min      2.313
_cell_volume                     4032.9(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      223.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0577
_diffrn_reflns_av_unetI/netI     0.0521
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            78016
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.032
_diffrn_reflns_theta_min         1.888
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.120
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6650
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.wR2(int) was 0.0762 before and 0.0645 after correction. The Ratio of minimum to maximum transmission is 0.8913. The \l/2 correction factor is 0.00150.'
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1880
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.834
_refine_diff_density_min         -0.733
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.406(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         11689
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0347
_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^)+(0.0293P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0642
_refine_ls_wR_factor_ref         0.0706
_reflns_Friedel_coverage         0.951
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                8962
_reflns_number_total             11689
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b08704_si_002.cif
_cod_data_source_block           Ba-macropa
_cod_database_code               4133153
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.946
_shelx_estimated_absorpt_t_min   0.767
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.594(14) 0.406(14)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 O8-H8
 0.83 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(O13A) = Uanis(O13B) = Uanis(O11A) = Uanis(O11B)
5. Others
 Sof(O11A)=Sof(O13A)=1-FVAR(1)
 Sof(O13B)=Sof(O11B)=FVAR(1)
6.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), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
 C12(H12A,H12B), C13(H13A,H13B), C20(H20A,H20B), C31(H31A,H31B), C32(H32A,H32B)
6.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C16(H16), C17(H17), C22(H22), C23(H23), C24(H24), C27(H27)
6.c Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C33(H33A,H33B,
 H33C)
;
_shelx_res_checksum              282
_shelx_hkl_checksum              74945
_olex2_submission_special_instructions 'No special instructions were received'