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_7059053
_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
'2(As H2 O4), As H3 O4, 4(C F3 O3 S), 3(H2 O), C27 H55 N14'
_chemical_formula_sum            'C31 H68 As3 F12 N14 O27 S4'
_chemical_formula_weight         1649.99
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2019-03-12
_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                96.081(3)
_cell_angle_beta                 90.171(3)
_cell_angle_gamma                109.012(3)
_cell_formula_units_Z            2
_cell_length_a                   12.6927(4)
_cell_length_b                   15.1722(5)
_cell_length_c                   17.0426(5)
_cell_measurement_reflns_used    9451
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      27.2210
_cell_measurement_theta_min      3.5520
_cell_volume                     3083.05(18)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.825
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset, Sapphire3'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_av_unetI/netI     0.0572
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.825
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            22380
_diffrn_reflns_point_group_measured_fraction_full 0.641
_diffrn_reflns_point_group_measured_fraction_max 0.524
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.935
_diffrn_reflns_theta_min         3.348
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.878
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92932
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.777
_exptl_crystal_description       block
_exptl_crystal_F_000             1678
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.605
_refine_diff_density_min         -1.103
_refine_diff_density_rms         0.127
_refine_ls_abs_structure_details
;
 Flack x determined using 2869 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.063(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1735
_refine_ls_number_reflns         15491
_refine_ls_number_restraints     104
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0628
_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^)+(0.0715P)^2^+12.3248P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1351
_refine_ls_wR_factor_ref         0.1420
_reflns_Friedel_coverage         0.270
_reflns_Friedel_fraction_full    0.290
_reflns_Friedel_fraction_max     0.223
_reflns_number_gt                13989
_reflns_number_total             15491
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj05231c2.cif
_cod_data_source_block           crystal7_arsen
_cod_original_cell_volume        3083.06(18)
_cod_database_code               7059053
_shelx_shelxl_version_number     2018/3
_exptl_absorpt_special_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_olex2_refinement_description
;
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
 C60-F61 = C60-F63 = C60-F62
 1.322 with sigma of 0.015
 S6-C60
 1.814 with sigma of 0.017
 O85_$1-H2E
 3.1 with sigma of 0.1
 O47_$2-H1D
 2.11 with sigma of 0.1
 O25_$1-H1C
 1.76 with sigma of 0.1
 H2F-O1_$3
 1.9 with sigma of 0.1
 H4A-N17_$4
 2.24 with sigma of 0.1
 O6-H5D
 2.4 with sigma of 0.1
 O15-H5C
 2.1 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
Uanis(O54) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C62) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(S8) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O87) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O75A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(F72B) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(F71B) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C61B) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(S7B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O76B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O77B) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(F73B) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(O75B) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(O76A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C41) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(S7B)=Sof(O75B)=Sof(O76B)=Sof(O77B)=Sof(C61B)=Sof(F72B)=Sof(F71B)=
 Sof(F73B)=1-FVAR(1)
 Sof(S7A)=Sof(F72A)=Sof(F73A)=Sof(F71A)=Sof(O77A)=Sof(O75A)=Sof(O76A)=
 Sof(C61A)=FVAR(1)
 Sof(O67B)=Sof(O65B)=Sof(O66B)=1-FVAR(2)
 Sof(O66A)=Sof(O67A)=Sof(O65A)=FVAR(2)
5.a Free rotating group:
 S8(O87,O85,O86,C62,F83,F82,F81), O4(H4A,H4B), O2(H2E,H2F), O5(H5C,H5D),
 O3(H3C,H3D), O1(H1C,H1D), O6(H6A,H6B), S7B(O75B,O76B,O77B,C61B,F72B,F71B,F73B)
5.b Ternary CH refined with riding coordinates:
 N1(H1), N20(H20)
5.c Secondary CH2 refined with riding coordinates:
 N14(H14A,H14B), N11(H11A,H11B), N5(H5A,H5B), N10(H10A,H10B), N2(H2A,H2B),
 N7(H7A,H7B), C20(H20A,H20B), C18(H18A,H18B), C17(H17A,H17B), C12(H12A,H12B),
 C27(H27A,H27B), C3(H3A,H3B), C9(H9A,H9B), C7(H7C,H7D), C8(H8A,H8B), C16(H16A,
 H16B), C19(H19A,H19B), C2(H2C,H2D), C21(H21A,H21B), C26(H26A,H26B), C25(H25A,
 H25B), C1(H1A,H1B), C11(H11C,H11D), C10(H10C,H10D), N19(H19C,H19D), N21(H21C,
 H21D), N25(H25C,H25D), N28(H28A,H28B), N24(H24A,H24B), N16(H16C,H16D),
 C35(H35A,H35B), C48(H48A,H48B), C45(H45A,H45B), C39(H39A,H39B), C47(H47A,H47B),
  C28(H28C,H28D), C36(H36A,H36B), C54(H54A,H54B), C38(H38A,H38B), C43(H43A,
 H43B), C44(H44A,H44B), C46(H46A,H46B), C53(H53A,H53B), C37(H37A,H37B),
 C52(H52A,H52B), C29(H29A,H29B), C34(H34A,H34B), C30(H30A,H30B)
5.d Aromatic/amide H refined with riding coordinates:
 N4(H4), N13(H13), N9(H9), C14(H14), C23(H23), C5(H5), N23(H23A), N18(H18),
 N27(H27), C32(H32), C41(H41), C50(H50)
5.e Tetrahedral OH refined with riding coordinates:
 O21(H21)
5.f Idealised tetrahedral OH refined as rotating group:
 O22(H22), O31(H31), O32(H32A), O33(H33), O11(H11), O12(H12), O41(H41A),
 O42(H42), O52(H52), O51(H51), O61(H61), O62(H62), O63(H63)
;
_shelx_res_checksum              99067
_olex2_submission_special_instructions 'No special instructions were received'