"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_7033563
_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 Cl2 Cu6 N28,2(C4H5N3O),4(Cl),10.166(H2O),4.18(O)'
_chemical_formula_sum            'C62 H120.33 Cl6 Cu6 N34 O16.35'
_chemical_formula_weight         2197.74
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_audit_update_record
;
2014-12-29 deposited with the CCDC.
2015-01-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.390(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.2950(7)
_cell_length_b                   12.2060(4)
_cell_length_c                   23.1240(10)
_cell_measurement_reflns_used    9842
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     4860.0(3)
_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, et al. J. Appl. Cryst. (2009).
;
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    Sir97
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.978
_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  0.0329
_diffrn_reflns_av_unetI/netI     0.0530
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            19352
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.467
_diffrn_reflns_theta_min         2.045
_exptl_absorpt_coefficient_mu    1.528
_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    1.502
_exptl_crystal_description       block
_exptl_crystal_F_000             2274.2
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_crystal_size_rad          0.3500
_refine_diff_density_max         1.003
_refine_diff_density_min         -0.929
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     626
_refine_ls_number_reflns         10887
_refine_ls_number_restraints     94
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1061
_refine_ls_R_factor_gt           0.0677
_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^)+(0.1287P)^2^+7.3403P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1967
_refine_ls_wR_factor_ref         0.2239
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7037
_reflns_number_total             10887
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt03650f2.cif
_cod_data_source_block           COMPOUND_4
_cod_depositor_comments
'Adding full bibliography for 7033560--7033563.cif.'
_cod_database_code               7033563
_shelx_shelxl_version_number     2013-4
_exptl_absorpt_correction_t_ave  0.4405