From isolated 1H-pyrazole cryptand anion receptors to hybrid inorganic-organic 1D helical polymeric anion receptors.
Pitarch-Jarque, Javier; Belda, Raquel; García-España, Laura; Llinares, José M; Pan, FangFang; Rissanen, Kari; Navarro, Pilar; García-España, Enrique; Dalton transactions (Cambridge, England : 2003) 44 (2015) 7761–7764; doi:10.1039/c5dt00763a

data_7034600
_publ_section_title
;
 From isolated 1H-pyrazole cryptand anion receptors to hybrid
 inorganic-organic 1D helical polymeric anion receptors.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7761
_journal_page_last               7764
_journal_paper_doi               10.1039/c5dt00763a
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C27 H54 N14, 6(Cl), 8(H2 O)'
_chemical_formula_sum            'C27 H70 Cl6 N14 O8'
_chemical_formula_weight         931.67
_chemical_name_systematic        'compound 3'
_chemical_properties_physical    Hygroscopic
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_update_record
;
2014-10-23 deposited with the CCDC.
2015-03-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 121.047(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.1190(8)
_cell_length_b                   15.1510(5)
_cell_length_c                   24.8700(11)
_cell_measurement_reflns_used    7358
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      0.998
_cell_volume                     4558.0(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, 2008)'
_computing_structure_solution
'SUPERFLIP, J. Appl. Cryst. (2007) 40, 786-790'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_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  0.0579
_diffrn_reflns_av_unetI/netI     0.0798
_diffrn_reflns_Laue_measured_fraction_full 0.960
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            14111
_diffrn_reflns_point_group_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         24.798
_diffrn_reflns_theta_min         1.912
_exptl_absorpt_coefficient_mu    0.435
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_description       block
_exptl_crystal_F_000             1984
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: H2O'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.644
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     530
_refine_ls_number_reflns         7709
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1266
_refine_ls_R_factor_gt           0.0626
_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^)+(0.0671P)^2^+4.7280P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1369
_refine_ls_wR_factor_ref         0.1712
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4445
_reflns_number_total             7709
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt00763a2.cif
_cod_data_source_block           COMPOUND3
_cod_depositor_comments
'Adding full bibliography for 7034599--7034600.cif.'
_cod_database_code               7034600
_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, All
  O(H,H) groups, All O(H,H,H,H) groups
2. Restrained distances
 H8C-O8
 0.82 with sigma of 0.02
 H8D-O8
 0.83 with sigma of 0.02
 H3C-O3
 0.82 with sigma of 0.02
 H3D-O3
 0.82 with sigma of 0.02
 H9C-O9
 0.82 with sigma of 0.02
 H9D-O9
 0.82 with sigma of 0.02
 H6A-O6
 0.82 with sigma of 0.02
 H6B-O6
 0.82 with sigma of 0.02
 H4A-O4
 0.82 with sigma of 0.02
 H4B-O4
 0.82 with sigma of 0.02
 H5C-O5
 0.82 with sigma of 0.02
 H5D-O5
 0.82 with sigma of 0.02
 H7E-O7
 0.82 with sigma of 0.02
 H7F-O7
 0.82 with sigma of 0.02
 H26A-H10C
 2.1 with sigma of 0.02
 O5-H5C
 0.82 with sigma of 0.02
 O5-H5D
 0.82 with sigma of 0.02
 HW2B-OW2
 0.82 with sigma of 0.02
 HW2A-OW2
 0.82 with sigma of 0.02
 HW1A-OW1
 0.82 with sigma of 0.02
 HW1B-OW1
 0.82 with sigma of 0.02
3. Rigid bond restraints
 C12, C13, C14, C15
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
N7 \\sim C13 \\sim C12: within 1.7A with sigma of 0.005 and sigma for terminal
atoms of 0.03
5. Others
 Fixed Sof: O9(0.7) H9C(0.7) H9D(0.7) O8(0.3) H8C(0.3) H8D(0.3)
6.a Rotating group with stretchable bonds:
 O7(H7E,H7F), OW1(HW1A,HW1B), OW2(HW2A,HW2B), O4(H4A,H4B), O5(H5C,H5D), O6(H6A,
 H6B), O9(H9C,H9D), O8(H8C,H8D), O3(H3C,H3D)
6.b Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), N7(H7A,H7B), N11(H11A,H11B), N10(H10A,H10B), N5(H5A,H5B),
 N14(H14A,H14B), C8(H8A,H8B), C19(H19A,H19B), C1(H1A,H1B), C3(H3A,H3B),
 C18(H18A,H18B), C2(H2C,H2D), C16(H16A,H16B), C27(H27A,H27B), C17(H17A,H17B),
 C26(H26A,H26B), C20(H20A,H20B), C9(H9A,H9B), C25(H25A,H25B), C7(H7C,H7D),
 C11(H11C,H11D), C21(H21A,H21B), C12(H12A,H12B)
6.c Secondary CH2 refined with riding coordinates and stretchable bonds:
 C10(H10C,H10D)
6.d Aromatic/amide H refined with riding coordinates:
 N13(H13), C5(H5), C23(H23), C14(H14)
;