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_7059054
_publ_section_title
;
 Water and Oxoanion Encapsulation Chemistry in a 1H-Pyrazole azacryptand
;
_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         '7(Cl O4), C27 H55 N14, 4(H2 O)'
_chemical_formula_sum            'C27 H63 Cl7 N14 O32'
_chemical_formula_weight         1344.06
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2019-03-11
_audit_creation_method
;
Olex2 1.2
(compiled May 29 2018 13:30:08 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-04-26 deposited with the CCDC.	2019-11-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.8160(10)
_cell_length_b                   13.9700(10)
_cell_length_c                   28.6830(10)
_cell_measurement_reflns_used    22979
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     5536.1(6)
_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)'
_computing_structure_solution    'SIR2011 (Burla et al.,  2007)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.998
_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  0.0941
_diffrn_reflns_av_unetI/netI     0.0830
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            43512
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.453
_diffrn_reflns_theta_min         1.420
_exptl_absorpt_coefficient_mu    0.463
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.613
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2792
_refine_diff_density_max         0.774
_refine_diff_density_min         -0.549
_refine_diff_density_rms         0.144
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.58(14)
_refine_ls_extinction_coef       0.0088(15)
_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   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     738
_refine_ls_number_reflns         12640
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1542
_refine_ls_R_factor_gt           0.0923
_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^)+(0.1840P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2567
_refine_ls_wR_factor_ref         0.2928
_reflns_Friedel_coverage         0.818
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                6890
_reflns_number_total             12640
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj05231c2.cif
_cod_data_source_block           crystal6_percl
_cod_database_code               7059054
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.42(14)
 0.58(14)
2. 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,H) groups
3. Restrained distances
 H1C-O24_$1
 2.2 with sigma of 0.1
 N3_$3-H3C
 1.8 with sigma of 0.1
 O3-H3C = O3-H3D
 0.85 with sigma of 0.02
 O43_$4-H3D
 2.2 with sigma of 0.1
 H3C-H3D
 1.33 with sigma of 0.02
4.a Free rotating group:
 O2(H2E,H2F), O1(H1C,H1D), O4(H4A,H4B)
4.b Ternary CH refined with riding coordinates:
 N1(H1)
4.c Secondary CH2 refined with riding coordinates:
 N14(H14A,H14B), N5(H5A,H5B), N11(H11A,H11B), N2(H2A,H2B), N10(H10A,H10B),
 N7(H7A,H7B), C26(H26A,H26B), C3(H3A,H3B), C8(H8A,H8B), C20(H20A,H20B), C2(H2C,
 H2D), C7(H7C,H7D), C25(H25A,H25B), C21(H21A,H21B), C17(H17A,H17B), C9(H9A,H9B),
  C27(H27A,H27B), C10(H10C,H10D), C12(H12A,H12B), C11(H11C,H11D), C16(H16A,
 H16B), C19(H19A,H19B), C1(H1A,H1B), C18(H18A,H18B)
4.d Aromatic/amide H refined with riding coordinates:
 N12(H12), N4(H4), C23(H23), C5(H5), N9(H9), C14(H14)
;
_shelx_res_checksum              69484
_olex2_submission_special_instructions 'No special instructions were received'