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_7059051
_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 H54 N14, 6(N O3), 5(H2 O)'
_chemical_formula_sum            'C27 H64 N20 O23'
_chemical_formula_weight         1036.98
_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             2019-01-18
_audit_creation_method
;
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                 114.465(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.1317(8)
_cell_length_b                   13.6910(6)
_cell_length_c                   19.6870(8)
_cell_measurement_reflns_used    16386
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      0.998
_cell_volume                     4693.7(4)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0736
_diffrn_reflns_av_unetI/netI     0.0668
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            28873
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         1.872
_exptl_absorpt_coefficient_mu    0.127
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_description       block
_exptl_crystal_F_000             2200
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.324
_refine_diff_density_min         -0.278
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       0.0088(9)
_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    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     690
_refine_ls_number_reflns         8257
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1368
_refine_ls_R_factor_gt           0.0594
_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^)+(0.1039P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1472
_refine_ls_wR_factor_ref         0.1939
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4071
_reflns_number_total             8257
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj05231c2.cif
_cod_data_source_block           crystal2_nitrate
_cod_original_cell_volume        4693.7(3)
_cod_database_code               7059051
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.989
_shelx_estimated_absorpt_t_min   0.985
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H2E,H2F} of O2, {H3C,H3D} of O3, {H4A,H4B} of O4, {H5C,
  H5D} of O5, All C(H,H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  {H1C,H1D} of O1
2. Restrained distances
 O2-H2E = O2-H2F
 0.82 with sigma of 0.02
 O3-H3C = O3-H3D
 0.82 with sigma of 0.02
 O4-H4A = O4-H4B
 0.82 with sigma of 0.02
 O5-H5C = O5-H5D
 0.82 with sigma of 0.02
 O11B-N1N
 1.3 with sigma of 0.01
 H2E-H2F
 1.33 with sigma of 0.04
 H3C-H3D
 1.33 with sigma of 0.04
 H4A-H4B
 1.33 with sigma of 0.04
 H5C-H5D
 1.33 with sigma of 0.04
 O22-N2N \\sim O21-N2N \\sim O23-N2N
 with sigma of 0.02
 O0AA-O1AA \\sim O1AA-O21 \\sim O0AA-O21
 with sigma of 0.02
3. Rigid bond restraints
 N1N, O11A
 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(O11A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.01
5. Others
 Sof(O13B)=Sof(O11B)=Sof(O12B)=1-FVAR(1)
 Sof(O11A)=Sof(O13A)=Sof(O12A)=FVAR(1)
 Sof(O1AA)=Sof(O0AA)=1-FVAR(2)
 Sof(O22)=Sof(O23)=FVAR(2)
6.a Free rotating group:
 O1(H1C,H1D)
6.b Rotating group with stretchable bonds:
 O2(H2E,H2F), O3(H3C,H3D), O4(H4A,H4B), O5(H5C,H5D)
6.c Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B),
 C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C16(H16A,H16B), C17(H17A,H17B),
  C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C25(H25A,
 H25B), C26(H26A,H26B), C27(H27A,H27B), N2(H2C,H2D), N5(H5A,H5B), N7(H7C,H7D),
 N10(H10C,H10D), N11(H11C,H11D), N14(H14A,H14B)
6.d Aromatic/amide H refined with riding coordinates:
 C5(H5), C14(H14), C23(H23), N4(H4), N9(H9), N13(H13)
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_shelx_res_checksum              80355
_olex2_submission_special_instructions 'No special instructions were received'