"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_7033562
_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_formula_moiety         'C54 H90 Cu6 N28, 6(N O3), 2(H2 O)'
_chemical_formula_sum            'C54 H94 Cu6 N34 O20'
_chemical_formula_weight         1920.87
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2bc 2ac'
_space_group_name_H-M_alt        'P c a b'
_symmetry_space_group_name_Hall  '-P 2bc 2ac'
_symmetry_space_group_name_H-M   'P c a b'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.5070(4)
_cell_length_b                   12.2300(2)
_cell_length_c                   20.9780(3)
_cell_measurement_reflns_used    15441
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     7570.34(19)
_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
;
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    SIR97
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_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  0.0501
_diffrn_reflns_av_unetI/netI     0.0420
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            29520
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.465
_diffrn_reflns_theta_min         2.371
_exptl_absorpt_coefficient_mu    1.748
_exptl_absorpt_correction_T_max  0.6090
_exptl_absorpt_correction_T_min  0.6044
_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    1.685
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             3960
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_exptl_crystal_size_rad          0.2000
_refine_diff_density_max         0.859
_refine_diff_density_min         -0.587
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     570
_refine_ls_number_reflns         8477
_refine_ls_number_restraints     80
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0770
_refine_ls_R_factor_gt           0.0428
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0645P)^2^+3.4448P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1101
_refine_ls_wR_factor_ref         0.1255
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5576
_reflns_number_total             8477
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt03650f2.cif
_cod_data_source_block           Compound_3
_cod_depositor_comments
'Adding full bibliography for 7033560--7033563.cif.'
_cod_database_code               7033562
_shelxl_version_number           2013-4
_exptl_absorpt_correction_t_ave  0.6070
_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
2. Restrained distances
 O1W-H1WA
 0.82 with sigma of 0.02
 O1W-H1WB
 0.82 with sigma of 0.02
3. Rigid bond restraints
 N1, C18
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N3N, O31B, O33B, O33A, O32B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.001
 C19, N1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N3N, O32A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N1N, O13A, O13B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O11A \\sim N1N: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
N1 \\sim C18: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
O23 \\sim O22 \\sim N2N \\sim O21: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.04
C4 \\sim N2 \\sim C3: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.01
N5 \\sim C6 \\sim C7: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.01
Uanis(O12A) \\sim Ueq, Uanis(O12B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5. Others
 Fixed Sof: O12A(0.5) O11A(0.5) O13A(0.5) O12B(0.5) O11B(0.5) O13B(0.5)
 O32B(0.5) O33B(0.5) O31B(0.5) O31A(0.5) O33A(0.5) O32A(0.5)
6.a Rotating group with stretchable bonds:
 O1W(H1WA,H1WB)
6.b Ternary CH refined with riding coordinates:
 N14(H14), N10(H10), N5(H5), N7(H7), N11(H11), N2(H2)
6.c Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C17(H17A,H17B), C8(H8A,H8B), C9(H9A,H9B), C12(H12A,H12B),
 C27(H27A,H27B), C16(H16A,H16B), C25(H25A,H25B), C11(H11A,H11B), C10(H10A,H10B),
  C26(H26A,H26B), C20(H20A,H20B), C18(H18A,H18B), C7(H7A,H7B), C19(H19A,H19B),
 C2(H2A,H2B), C3(H3A,H3B), C1(H1A,H1B)
6.d Aromatic/amide H refined with riding coordinates:
 C23(H23), C5(H5A), C14(H14A)
;