"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_7033560
_publ_section_title
;
 &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_absolute_configuration unk
_chemical_formula_moiety         'C27 H46 Cu2 N14, 2(Cl O4), 2(H2 O)'
_chemical_formula_sum            'C27 H50 Cl2 Cu2 N14 O10'
_chemical_formula_weight         928.79
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2014-01-20
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_audit_update_record
;
2014-11-18 deposited with the CCDC.
2015-01-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.552(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.3240(4)
_cell_length_b                   10.0650(3)
_cell_length_c                   15.2650(5)
_cell_measurement_reflns_used    4511
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     1891.61(10)
_computing_cell_refinement       'HKL Scalepack ,Otwinowski & Minor 1997.'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo & 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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0509
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_number            8541
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         24.993
_diffrn_reflns_theta_min         2.079
_exptl_absorpt_coefficient_mu    1.338
_exptl_absorpt_correction_T_max  0.5195
_exptl_absorpt_correction_T_min  0.5123
_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    1.631
_exptl_crystal_description       block
_exptl_crystal_F_000             964
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.465
_refine_diff_density_min         -0.387
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details
;
 Flack x determined using 2072 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.007(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     549
_refine_ls_number_reflns         6643
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0479
_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^)+(0.0489P)^2^+2.2814P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1043
_refine_ls_wR_factor_ref         0.1193
_reflns_Friedel_coverage         0.881
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                5281
_reflns_number_total             6643
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt03650f2.cif
_cod_data_source_block           Compound_1
_cod_depositor_comments
'Adding full bibliography for 7033560--7033563.cif.'
_cod_database_code               7033560
_shelxl_version_number           2013-4
_exptl_absorpt_correction_t_ave  0.5165
_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
2. Restrained distances
 O2-H2C = O2-H2D
 0.82 with sigma of 0.02
 O1-H1C = O1-H1D
 0.82 with sigma of 0.02
 N11-H11
 0.9 with sigma of 0.02
 H14-N14
 0.9 with sigma of 0.02
 H16B-H17B
 2.2 with sigma of 0.01
 C18-C17
 1.5 with sigma of 0.02
 C18B-C17B
 1.5 with sigma of 0.02
3. Rigid bond restraints
 N10, C16
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C5, C6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C10, C11
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cl2, O22
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C13 \\sim C12: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.04
C15 \\sim C16 \\sim C18 \\sim C17 \\sim N10: within 1.7A with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C17) \\sim Ueq: with sigma of 0.008 and sigma for terminal atoms of 0.2
Uanis(C16) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
5. Others
 Fixed Sof: H10(0.5) H10A(0.5) C18(0.5) H18A(0.5) H18B(0.5) O23(0.5) O22(0.5)
 O21(0.5) C17(0.5) H17A(0.5) H17B(0.5) C18B(0.5) H18C(0.5) H18D(0.5) O23B(0.5)
 O22B(0.5) O21B(0.5) C17B(0.5) H17C(0.5) H17D(0.5)
6.a Riding coordinates:
 N2(H2), N13(H13), C25(H25A,H25B), N5(H5), C21(H21A,H21B), C14(H14A), C20(H20A,
 H20B), C23(H23), C1(H1A,H1B), C19(H19A,H19B), N7(H7), C26(H26A,H26B), C2(H2A,
 H2B), C11(H11A,H11B), C5(H5A), C9(H9A,H9B), C27(H27A,H27B), C3(H3A,H3B),
 C10(H10B,H10C), C12(H12A,H12B), C7(H7A,H7B), C16(H16A,H16B)
6.b Rotating group with stretchable bonds:
 N11(H11), N14(H14), O2(H2C,H2D), O1(H1C,H1D)
6.c Ternary CH refined with riding coordinates:
 N10(H10), N10(H10A)
6.d Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C18(H18A,H18B), C17(H17A,H17B), C18B(H18C,H18D), C17B(H17C,H17D)
;