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_7034599
_publ_section_title
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 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
'2(C108 H216 Cl18 Cu6 N56), 36(Cl), 24(H2 O), 49(O), H4 O4'
_chemical_formula_sum            'C216 H484 Cl72 Cu12 N112 O77'
_chemical_formula_weight         9198.00
_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_creation_date             2014-01-24
_audit_creation_method
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_audit_update_record
;
2014-11-09 deposited with the CCDC.
2015-03-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 132.674(6)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   20.6746(7)
_cell_length_b                   18.6770(3)
_cell_length_c                   40.0092(14)
_cell_measurement_reflns_used    23917
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      76.0810
_cell_measurement_theta_min      4.0650
_cell_volume                     11358.5(12)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SIR 97'
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector_area_resol_mean 5.1977
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0239
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            49666
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.000
_diffrn_reflns_theta_max         67.00
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    5.084
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47031
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_description       block
_exptl_crystal_F_000             4751.9
_exptl_crystal_size_max          0.3525
_exptl_crystal_size_mid          0.1741
_exptl_crystal_size_min          0.0620
_refine_diff_density_max         1.983
_refine_diff_density_min         -1.315
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.542
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1254
_refine_ls_number_reflns         20216
_refine_ls_number_restraints     281
_refine_ls_restrained_S_all      1.539
_refine_ls_R_factor_all          0.1049
_refine_ls_R_factor_gt           0.0975
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3214
_refine_ls_wR_factor_ref         0.3382
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17539
_reflns_number_total             20216
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt00763a2.cif
_cod_data_source_block           COMPOUND4
_cod_depositor_comments
'Adding full bibliography for 7034599--7034600.cif.'
_cod_original_cell_volume        11358.6(12)
_cod_database_code               7034599
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H19E,H19F} of O19, All C(H,H) groups, All N(H) groups,
  All N(H,H) groups
 At 1.5 times of:
  {H3C,H3D} of O3, {H5C,H5D} of O5, {H1C,H1D} of O1, {H2E,H2F} of O2, {H27C,
  H27D} of O27, {H4A,H4B} of O4
2. Restrained distances
 C1-C2
 1.55 with sigma of 0.02
 O2-H2F
 0.82 with sigma of 0.02
 H2E-O2
 0.82 with sigma of 0.02
 H5D-O5
 0.82 with sigma of 0.02
 O5-H5C
 0.82 with sigma of 0.02
 H5D-H24A
 2.18 with sigma of 0.001
 H2F-H11A
 2.18 with sigma of 0.02
 O19-H19F
 0.82 with sigma of 0.02
 O19-H19E
 0.82 with sigma of 0.02
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C2 \\sim C1: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
C4 \\sim C3: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(O20) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
5. Others
 Fixed Sof: Cl13(0.5) Cl15(0.5) O31(0.5) Cl18(0.5) Cl14(0.5) Cl22(0.33333)
 O19(0.5) H19E(0.5) H19F(0.5) Cl19(0.33333) Cl23(0.33333) Cl24(0.33333)
 O10(0.5) O11(0.5) Cl21(0.33335) Cl20(0.33333) O9(0.5) O12(0.5) O13(0.5)
 O8(0.5) O14(0.5) O20(0.75) O15(0.5) O23(0.5) O16(0.5) O22(0.5) O24(0.5)
 O18(0.5) O1A(0.5) O26(0.5) O21(0.5) O1D(0.5)
6.a Free rotating group:
 O3(H3C,H3D,O5,H5C,H5D,O1,H1C,H1D), O27(H27C,H27D), O4(H4A,H4B)
6.b Rotating group with stretchable bonds:
 O19(H19E,H19F)
6.c Secondary CH2 refined with riding coordinates:
 N16(H16A,H16B), C37(H37A,H37B), N10(H10A,H10B), N5(H5A,H5B), C25(H25A,H25B),
 N19(H19A,H19B), N24(H24A,H24B), C54(H54A,H54B), N11(H11A,H11B), C38(H38A,H38B),
  C53(H53A,H53B), C26(H26A,H26B), C18(H18A,H18B), N14(H14A,H14B), N28(H28A,
 H28B), N7(H7A,H7B), C21(H21A,H21B), C28(H28C,H28D), C36(H36A,H36B), C10(H10C,
 H10D), C29(H29A,H29B), C52(H52A,H52B), C9(H9A,H9B), N21(H21C,H21D), C19(H19C,
 H19D), C8(H8A,H8B), C16(H16C,H16D), N25(H25C,H25D), C11(H11C,H11D), C2(H2A,
 H2B), C34(H34A,H34B), C12(H12A,H12B), C20(H20A,H20B), C43(H43A,H43B), N2(H2C,
 H2D), C17(H17A,H17B), C27(H27A,H27B), C30(H30A,H30B), C44(H44A,H44B), C45(H45A,
 H45B), C47(H47A,H47B), C39(H39A,H39B), C7(H7C,H7D), C48(H48A,H48B), C46(H46A,
 H46B), C35(H35A,H35B), C3(H3A,H3B), C1(H1A,H1B)
6.d Aromatic/amide H refined with riding coordinates:
 N27(H27), C5(H5), N13(H13), C32(H32), N9(H9), C50(H50), N17(H17), N4(H4),
 C14(H14), N23(H23), C23(H23A), C41(H41)
;
_smtbx_masks_special_details
;
Diffuse, disordered solvent molecules could not be adequately modeled.The
bypass procedure Solvent Mask from Olex2 software was used to remove the
electronic contribution from
these solvents. The total potential solvent accessible void volume
 was 687 Ang^3^ and the electron count / cell = 62.4. As the exact 
solvent content is not known, the reported formula reflects only the 
atoms used in the refinement. 
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