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_7059050
_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 H50 N14, 2.65(H2 O), 2(Cl O4)'
_chemical_formula_sum            'C27 H55.31 Cl2 N14 O10.65'
_chemical_formula_weight         817.54
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-04-02
_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                94.242(2)
_cell_angle_beta                 103.849(2)
_cell_angle_gamma                111.844(2)
_cell_formula_units_Z            2
_cell_length_a                   10.5140(3)
_cell_length_b                   13.1320(5)
_cell_length_c                   15.7580(6)
_cell_measurement_reflns_used    7859
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.373
_cell_measurement_theta_min      0.998
_cell_volume                     1928.43(12)
_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(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0489
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6772
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.031
_diffrn_reflns_theta_max         25.031
_diffrn_reflns_theta_min         1.699
_exptl_absorpt_coefficient_mu    0.241
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_description       block
_exptl_crystal_F_000             869
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.288
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     626
_refine_ls_number_reflns         6772
_refine_ls_number_restraints     68
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0891
_refine_ls_R_factor_gt           0.0560
_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^)+(0.0556P)^2^+0.9356P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1257
_refine_ls_wR_factor_ref         0.1416
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4619
_reflns_number_total             6772
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj05231c2.cif
_cod_data_source_block           crystal1
_cod_database_code               7059050
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.960
_shelx_estimated_absorpt_t_min   0.931
_olex2_refinement_description
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1. Twinned data refinement
 Scales: 0.844(2)
 0.156(2)
2. Fixed Uiso
 At 1.2 times of:
  All H(H,H,H) groups, {H4A,H4B} of O4, All C(H) groups, All C(H,H) groups,
  All N(H) groups
 At 1.5 times of:
  {H1C,H1D} of O1, {H3C,H3D} of O3, {H2C,H2D} of O2
3. Restrained distances
 H4B-O24_$1
 1.6 with sigma of 0.1
 H4A-O21_$2
 2 with sigma of 0.1
 Cl2A-O21 \\sim Cl2A-O22 \\sim Cl2A-O24 \\sim Cl2A-O23
 with sigma of 0.02
 O21-O22 \\sim O21-O24 \\sim O21-O23 \\sim O22-O24 \\sim O22-O23 \\sim O24-O23
 with sigma of 0.02
 Cl2B-O28 \\sim Cl2B-O27 \\sim Cl2B-O25 \\sim Cl2B-O26
 with sigma of 0.02
 O18-O17 \\sim O18-O16 \\sim O18-O15 \\sim O17-O16 \\sim O17-O15 \\sim O16-O15
 with sigma of 0.02
 Cl1-O17 \\sim Cl1-O16 \\sim Cl1-O15 \\sim Cl1-O18
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(O17) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(O15) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O12) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(Cl2B)=Sof(O28)=Sof(O27)=Sof(O26)=Sof(O25)=1-FVAR(1)
 Sof(Cl2A)=Sof(O22)=Sof(O21)=Sof(O24)=Sof(O23)=FVAR(1)
 Sof(O16)=Sof(O15)=Sof(O17)=Sof(O18)=1-FVAR(2)
 Sof(O14)=Sof(O11)=Sof(O12)=Sof(O13)=FVAR(2)
 Sof(O3)=Sof(H3C)=Sof(H3D)=FVAR(3)
 Sof(O4)=Sof(H4A)=Sof(H4B)=FVAR(4)
 Fixed Sof: H11(0.5) H5A(0.5)
6.a Free rotating group:
 O1(H1C,H1D), O2(H2C,H2D), O3(H3C,H3D), O4(H4A,H4B)
6.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C18(H18A,H18B), C16(H16A,H16B), C19(H19A,H19B), C3(H3A,H3B),
 C10(H10C,H10D), C20(H20A,H20B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B),
  C21(H21A,H21B), C17(H17A,H17B), C7(H7A,H7B), C1(H1A,H1B), C8(H8A,H8B), C9(H9A,
 H9B), C12(H12A,H12B), C11(H11B,H11C)
6.c Aromatic/amide H refined with riding coordinates:
 N13(H13), N3(H3), C23(H23), C14(H14A), C5(H5)
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_shelx_res_checksum              24131
_olex2_submission_special_instructions 'No special instructions were received'