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_7059052
_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         'C27 H58 N14, 11(H2 O4 P), 4(H2 O)'
_chemical_formula_sum            'C27 H88 N14 O48 P11'
_chemical_formula_weight         1717.78
_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
;
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                 112.3250(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.8632(2)
_cell_length_b                   20.1186(2)
_cell_length_c                   24.7970(4)
_cell_measurement_reflns_used    22633
_cell_measurement_temperature    288.15
_cell_measurement_theta_max      74.9314
_cell_measurement_theta_min      2.9192
_cell_volume                     6859.17(17)
_computing_cell_refinement
'CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42)'
_computing_data_collection
'CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42)'
_computing_data_reduction
'CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42)'
_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      288.15
_diffrn_detector_area_resol_mean 8.2640
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Xcalibur, Onyx, Nova'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0560
_diffrn_reflns_av_unetI/netI     0.0332
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            61232
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.483
_diffrn_reflns_theta_min         2.922
_exptl_absorpt_coefficient_mu    3.626
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74268
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET)
(compiled Sep 15 2009,11:49:04)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.663
_exptl_crystal_description       block
_exptl_crystal_F_000             3588
_exptl_crystal_size_max          0.2503
_exptl_crystal_size_mid          0.2091
_exptl_crystal_size_min          0.0728
_refine_diff_density_max         1.493
_refine_diff_density_min         -0.630
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1076
_refine_ls_number_reflns         14093
_refine_ls_number_restraints     105
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0884
_refine_ls_R_factor_gt           0.0741
_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^)+(0.1662P)^2^+2.3204P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2239
_refine_ls_wR_factor_ref         0.2432
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10750
_reflns_number_total             14093
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj05231c2.cif
_cod_data_source_block           crystal3_phos11
_cod_database_code               7059052
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.778
_shelx_estimated_absorpt_t_min   0.464
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H4A,H4B} of O4, H11 of O11, H12C of O12, H93 of O93, {H2E,
  H2F} of O2, H42 of O42, All C(H,H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  H7AA of O74, H73 of O73, H112 of O112, H51 of O51, H76 of O76, H115 of O115,
   H72 of O72, H22 of O22, H91 of O91, H77 of O77, H31 of O31, H11E of O117,
  H111 of O111, H32 of O32, H21 of O21, H7BB of O75, H56 of O56, H5BA of O57,
  H63 of O63, H81 of O81, H52 of O52, H92 of O92, H41 of O41, {H1AA,H1AB} of
  O1A, {H3C,H3D} of O3, H61 of O61, H102 of O102, {H1BA,H1BB} of O1B, H83 of
  O83, H101 of O101
2. Restrained distances
 O31-H3C
 2.1 with sigma of 0.1
 O94-H3D
 1.9 with sigma of 0.1
 H21-H3
 2.5 with sigma of 0.2
 O1B-H1BB = O1B-H1BA
 0.85 with sigma of 0.02
 H1BB-O56
 2 with sigma of 0.1
 O84_$1-H91
 1.7 with sigma of 0.1
 H1BA-O64
 2.4 with sigma of 0.1
 O111-O114 \\sim O111-O113 \\sim O111-O112 \\sim O114-O113 \\sim O114-O112
\\sim O113-O112
 with sigma of 0.05
 O116-O118 \\sim O116-O117 \\sim O116-O115 \\sim O118-O117 \\sim O118-O115
\\sim O117-O115
 with sigma of 0.05
3. Rigid bond restraints
 O55
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O116
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 P7, O71, O72, O75, O76
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
P3 \\sim O31 \\sim O34: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
P2 \\sim O21 \\sim O22: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Uanis(O114) \\sim Ueq, Uanis(O112) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(O58) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O55) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(O118) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O56) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(P11B)=Sof(O115)=Sof(H115)=Sof(O116)=Sof(O117)=Sof(H11E)=Sof(O118)=1-FVAR(1)
 Sof(P11A)=Sof(O111)=Sof(H111)=Sof(O112)=Sof(H112)=Sof(O113)=Sof(O114)=FVAR(1)
 Sof(O75)=Sof(O76)=Sof(O77)=1-FVAR(2)
 Sof(H7BB)=Sof(H76)=Sof(H77)=0.66667*(1-FVAR(3))
 Sof(H72)=Sof(H73)=Sof(H7AA)=0.66667*FVAR(3)
 Sof(O72)=Sof(O73)=Sof(O74)=FVAR(2)
 Sof(P5B)=Sof(O55)=Sof(O56)=Sof(H56)=Sof(O57)=Sof(H5BA)=Sof(O58)=1-FVAR(3)
 Sof(P5A)=Sof(O51)=Sof(H51)=Sof(O52)=Sof(H52)=Sof(O53)=Sof(O54)=FVAR(3)
 Sof(O1B)=Sof(H1BA)=Sof(H1BB)=1-FVAR(4)
 Sof(O1A)=Sof(H1AA)=Sof(H1AB)=FVAR(4)
 Fixed Sof: H91(0.66666) H92(0.66666) H93(0.66666)
6.a Free rotating group:
 O3(H3C,H3D), O1A(H1AA,H1AB), O2(H2E,H2F), O4(H4A,H4B)
6.b Rotating group with stretchable bonds:
 O42(H42), O1B(H1BA,H1BB)
6.c Ternary CH refined with riding coordinates:
 N1(H1), N6(H6)
6.d Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), N5(H5A,H5B), N7(H7A,H7B), N10(H10A,H10B), N11(H11A,H11B),
 N14(H14A,H14B), C2(H2C,H2D), C3(H3A,H3B), C7(H7C,H7D), C8(H8A,H8B), C9(H9A,
 H9B), C10(H10C,H10D), C11(H11C,H11D), 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)
6.e Aromatic/amide H refined with riding coordinates:
 N3(H3), N4(H4), N8(H8), N9(H9), N12(H12), N13(H13), C5(H5), C14(H14), C23(H23)
6.f Tetrahedral OH refined with riding coordinates:
 O117(H11E), O21(H21), O92(H92), O56(H56)
6.g Idealised tetrahedral OH refined as rotating group:
 O72(H72), O73(H73), O74(H7AA), O75(H7BB), O76(H76), O77(H77), O11(H11),
 O12(H12C), O115(H115), O22(H22), O31(H31), O32(H32), O91(H91), O93(H93),
 O111(H111), O112(H112), O51(H51), O52(H52), O61(H61), O63(H63), O57(H5BA),
 O41(H41), O81(H81), O83(H83), O101(H101), O102(H102)
;
_shelx_res_checksum              48600
_olex2_submission_original_sample_id phos11
_olex2_submission_special_instructions 'No special instructions were received'