Water and Oxoanion Encapsulation Chemistry in a 1H-Pyrazole azacryptand
Pitarch-Jarque, Javier; Rissanen, Kari; Garcia-Granda, Santiago; Lopera, Alberto; Clares, Maria Paz; García-España, Enrique; Blasco, Salvador; New Journal of Chemistry 43 (2019) 18915–18924; doi:10.1039/C9NJ05231C

data_7059055
_publ_section_title
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 Water and Oxoanion Encapsulation Chemistry in a 1H-Pyrazole azacryptand
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_journal_issue                   47
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              18915
_journal_page_last               18924
_journal_paper_doi               10.1039/C9NJ05231C
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety         'C27 H57 N14, 3(O4 S), 3(H O4 S), 6(H2 O)'
_chemical_formula_sum            'C27 H72 N14 O30 S6'
_chemical_formula_weight         1265.34
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-03-11
_audit_creation_method
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Olex2 1.2
(compiled May 29 2018 13:30:08 for OlexSys, GUI svn.r5506)
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_audit_update_record
;
2019-04-26 deposited with the CCDC.	2019-11-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.7130(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.4324(2)
_cell_length_b                   17.2812(3)
_cell_length_c                   26.4489(4)
_cell_measurement_reflns_used    20583
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.103
_cell_measurement_theta_min      0.998
_cell_volume                     5189.57(15)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      293.15
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0924
_diffrn_reflns_av_unetI/netI     0.0760
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            42829
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.453
_diffrn_reflns_theta_min         1.948
_exptl_absorpt_coefficient_mu    0.370
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_description       plate
_exptl_crystal_F_000             2672
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.466
_refine_diff_density_min         -0.512
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       0.0018(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     756
_refine_ls_number_reflns         11838
_refine_ls_number_restraints     53
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.1236
_refine_ls_R_factor_gt           0.0553
_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^)+(0.0793P)^2^+0.8105P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1309
_refine_ls_wR_factor_ref         0.1604
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6370
_reflns_number_total             11838
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj05231c2.cif
_cod_data_source_block           crystal5_sulphate
_cod_database_code               7059055
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.993
_shelx_estimated_absorpt_t_min   0.910
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 H3D-O51
 1.9 with sigma of 0.1
 O20_$6-H3C
 1.4 with sigma of 0.1
 O43-H2E
 2 with sigma of 0.1
 H4A-O3
 2 with sigma of 0.1
 O21-O24 \\sim O21-O25 \\sim O21-O20 \\sim O24-O25 \\sim O24-O20 \\sim O24-O21
 with sigma of 0.02
 S2A-O21 \\sim S2A-O24 \\sim S2A-O25 \\sim S2A-O20
 with sigma of 0.02
 O23-O22 \\sim O23-O27 \\sim O23-O26 \\sim O22-O27 \\sim O22-O26 \\sim O27-O26
 with sigma of 0.02
 S2B-O27 \\sim S2B-O22 \\sim S2B-O23 \\sim S2B-O26
 with sigma of 0.02
3. Rigid bond restraints
 S2B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(O26) \\sim Ueq, Uanis(O27) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
5. Others
 Sof(S2B)=Sof(O26)=Sof(O23)=Sof(O27)=Sof(O22)=1-FVAR(1)
 Sof(S2A)=Sof(O25)=Sof(O20)=Sof(O24)=Sof(O21)=FVAR(1)
 Fixed X: H1C(0.431409) H1D(0.432329) H3C(0.04363) H3D(0.08855)
 Fixed Y: H1C(0.29216) H1D(0.317361) H3C(0.06403) H3D(0.08434)
 Fixed Z: H1C(0.34235) H1D(0.287459) H3C(0.03868) H3D(0.086519)
6.a Free rotating group:
 O2(H2E,H2F), O4(H4A,H4B), O5(H5C,H5D), O6(H6A,H6B)
6.b Secondary CH2 refined with riding coordinates:
 N10(H10A,H10B), N2(H2A,H2B), N5(H5A,H5B), N14(H14A,H14B), N11(H11A,H11B),
 N7(H7A,H7B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C1(H1A,H1B),
 C2(H2C,H2D), C3(H3A,H3B), C7(H7C,H7D), C8(H8A,H8B), C9(H9A,H9B), C27(H27A,
 H27B), C26(H26A,H26B), C25(H25A,H25B), C21(H21A,H21B), C20(H20A,H20B),
 C19(H19A,H19B), C10(H10C,H10D), C11(H11C,H11D), C12(H12A,H12B)
6.c Aromatic/amide H refined with riding coordinates:
 N8(H8), N9(H9), N3(H3), N4(H4), N13(H13), N12(H12), C23(H23), C14(H14), C5(H5)
6.d Idealised tetrahedral OH refined as rotating group:
 O13(H13A), O54(H54), O63(H63)
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_shelx_res_checksum              47270
_olex2_submission_special_instructions 'No special instructions were received'