"3 + 1 = 6 + 2" in Cu(ii) coordination chemistry of 1H-pyrazole aza cryptands.
Pitarch-Jarque, Javier; Belda, Raquel; Lloret, Francesc; Ferrando-Soria, Jesús; Navarro, Pilar; Lopera, Alberto; García-España, Enrique; Dalton transactions (Cambridge, England : 2003) 44 (2015) 3378–3383; doi:10.1039/c4dt03650f

data_7033561
_publ_section_title
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 &quot;3 + 1 = 6 + 2&quot; in Cu(ii) coordination chemistry of 1H-pyrazole
 aza cryptands.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3378
_journal_page_last               3383
_journal_paper_doi               10.1039/c4dt03650f
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C54 H94 Cu6 N28 O2, 6(C7 H7 O3 S), 22(H2 O)'
_chemical_formula_sum            'C96 H180 Cu6 N28 O42 S6'
_chemical_formula_weight         2972.34
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2014-01-21
_audit_creation_method
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_audit_update_record
;
2014-11-18 deposited with the CCDC.
2015-01-06 downloaded from the CCDC.
;
_cell_angle_alpha                79.7500(10)
_cell_angle_beta                 76.0550(10)
_cell_angle_gamma                62.0960(10)
_cell_formula_units_Z            1
_cell_length_a                   12.6670(2)
_cell_length_b                   13.5270(3)
_cell_length_c                   21.6730(5)
_cell_measurement_reflns_used    14177
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     3175.90(12)
_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    sir92
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0358
_diffrn_reflns_av_unetI/netI     0.0502
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            21630
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.708
_exptl_absorpt_coefficient_mu    1.178
_exptl_absorpt_correction_T_max  0.4447
_exptl_absorpt_correction_T_min  0.4350
_exptl_absorpt_correction_type   cylinder
_exptl_absorpt_process_details
;
Interpolation using  Int.Tab. Vol. C (1992) p. 523,Tab. 6.3.3.3
for values of muR in the range 0-2.5, and Int.Tab. Vol.II (1959)
p.302; Table 5.3.6 B for muR in the range 2.6-10.0.
The interpolation procedure of C.W.Dwiggins Jr (Acta Cryst.(1975)
A31,146-148) is used with some modification.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_description       block
_exptl_crystal_F_000             1558
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_crystal_size_rad          0.4000
_refine_diff_density_max         1.407
_refine_diff_density_min         -1.279
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     842
_refine_ls_number_reflns         11150
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0501
_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^)+(0.0398P)^2^+10.4656P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1203
_refine_ls_wR_factor_ref         0.1258
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9032
_reflns_number_total             11150
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt03650f2.cif
_cod_data_source_block           COMPOUND_2
_cod_depositor_comments
'Adding full bibliography for 7033560--7033563.cif.'
_cod_database_code               7033561
_shelxl_version_number           2013-4
_exptl_absorpt_correction_t_ave  0.4405
_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 O(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H10C-O10
 0.82 with sigma of 0.02
 H10D-O10
 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
 H5C-O5
 0.82 with sigma of 0.02
 H5B-O5
 0.82 with sigma of 0.02
 H8D-O8
 0.82 with sigma of 0.02
 H8C-O8
 0.82 with sigma of 0.02
 O9-H9D
 0.82 with sigma of 0.02
 O9-H9C
 0.82 with sigma of 0.02
 H4A-O4
 0.82 with sigma of 0.02
 O4-H4B
 0.82 with sigma of 0.02
 O12-H12D
 0.82 with sigma of 0.02
 O12-H12C
 0.82 with sigma of 0.02
 H2D-O2
 0.82 with sigma of 0.02
 O2-H2C
 0.82 with sigma of 0.02
 H1A-O1
 0.82 with sigma of 0.02
 O11-H11D
 0.82 with sigma of 0.02
 H11C-O11
 0.82 with sigma of 0.02
 H13B-O13
 0.82 with sigma of 0.02
 O13-H13A
 0.82 with sigma of 0.02
 H7C-O7
 0.82 with sigma of 0.02
 O7-H7D
 0.82 with sigma of 0.02
 O10-O7
 2.5 with sigma of 0.01
 H3C-O3
 0.82 with sigma of 0.02
 H3D-O3
 0.82 with sigma of 0.02
3. Others
 Fixed Sof: O10(0.5) H10C(0.5) H10D(0.5) O3(0.5) H3C(0.5) H3D(0.5)
4.a Rotating group with stretchable bonds:
 O5(H5B,H5C), O1(H1A,H1B), O9(H9C,H9D), O4(H4A,H4B), O8(H8C,H8D), O2(H2C,H2D),
 O11(H11C,H11D), O13(H13A,H13B), O6(H6A,H6B), O12(H12C,H12D), O7(H7C,H7D),
 O10(H10C,H10D), O3(H3C,H3D)
4.b Ternary CH refined with riding coordinates:
 N10(H10)
4.c Ternary CH refined with riding coordinates and stretchable bonds:
 N5(H5), N11(H11), N14(H14), N7(H7), N2(H2)
4.d Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C19(H19A,H19B), C27(H27A,H27B), C9(H9A,H9B), C7(H7A,H7B),
 C21(H21A,H21B), C26(H26A,H26B), C25(H25A,H25B), C18(H18A,H18B), C8(H8A,H8B),
 C17(H17A,H17B), C16(H16A,H16B), C1(H1C,H1D), C11(H11A,H11B), C3(H3A,H3B),
 C2(H2A,H2B), C12(H12A,H12B), C20(H20A,H20B)
4.e Me refined with riding coordinates:
 C27T(H27C,H27D,H27E), C37T(H37A,H37B,H37C), C17T(H17C,H17D,H17E)
4.f Aromatic/amide H refined with riding coordinates:
 C23(H23), C15T(H15T), C16T(H16T), C14(H14A), C5(H5A), C33T(H33T), C13T(H13T),
 C12T(H12T), C26T(H26T), C32T(H32T), C36T(H36T), C35T(H35T), C25T(H25T),
 C22T(H22T), C23T(H23T)
;