#------------------------------------------------------------------------------
#$Date: 2016-03-25 15:54:39 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179942 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/37/7023755.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7023755
loop_
_publ_author_name
'Wang, Ling'
'Guo, Bin'
'Li, Hong-Xi'
'Li, Qi'
'Li, Hai-Yan'
'Lang, Jian-Ping'
_publ_section_title
;
 Polynuclear copper(ii) pyrazolate complexes: temperature-dependent
 protonolysis reactions, crystal structures and high catalytic activity
 toward the condensation of nitriles with 2-aminoalcohol.
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15570
_journal_page_last               15580
_journal_paper_doi               10.1039/c3dt51970h
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         '2(C28 H28 Cu4 N8 O20), 8(CH3OH), OH2'
_chemical_formula_sum            'C64 H90 Cu8 N16 O49'
_chemical_formula_weight         2375.84
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.5074(10)
_cell_length_b                   15.5074(10)
_cell_length_c                   19.8920(12)
_cell_measurement_reflns_used    9908
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.96
_cell_measurement_theta_min      2.63
_cell_volume                     4783.6(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0516
_diffrn_reflns_av_sigmaI/netI    0.0313
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            35860
_diffrn_reflns_theta_full        28.77
_diffrn_reflns_theta_max         28.77
_diffrn_reflns_theta_min         2.63
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.845
_exptl_absorpt_correction_T_max  0.7568
_exptl_absorpt_correction_T_min  0.6763
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2352
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.747
_refine_diff_density_min         -1.049
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     157
_refine_ls_number_reflns         3106
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0823
_refine_ls_R_factor_gt           0.0590
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1157P)²+24.4786P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1780
_refine_ls_wR_factor_ref         0.1991
_reflns_number_gt                2337
_reflns_number_total             3106
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt51970h.txt
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      I4(1)/a
_cod_database_code               7023755
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y+3/4, x+1/4, z+1/4'
'-x+1/2, -y, z+1/2'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'-x+1, -y+1/2, z+1'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'y-3/4, -x-1/4, -z-1/4'
'x-1/2, y, -z-1/2'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'x, y+1/2, -z'
'-y-1/4, x-1/4, -z-1/4'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.05585(3) 0.87975(3) 0.30688(2) 0.0248(2) Uani 1 1 d . . .
O1 O 0.1847(2) 0.9556(2) 0.34435(16) 0.0354(7) Uani 1 1 d . . .
O2 O 0.2359(2) 1.0009(3) 0.44313(16) 0.0410(9) Uani 1 1 d . . .
O3 O -0.1239(2) 0.8179(2) 0.54042(16) 0.0298(7) Uani 1 1 d . . .
O4 O -0.0496(2) 0.8828(2) 0.62235(15) 0.0338(7) Uani 1 1 d . . .
O5 O -0.0100(2) 0.9892(2) 0.30121(16) 0.0315(7) Uani 1 1 d D . .
H5 H 0.012(3) 1.025(3) 0.329(2) 0.038 Uiso 1 1 d D . .
O7 O 0.0000 0.2500 0.1250 0.120(10) Uiso 0.50 4 d SP . .
N1 N 0.0460(2) 0.8842(2) 0.40566(18) 0.0238(7) Uani 1 1 d . . .
N2 N -0.0154(2) 0.8581(2) 0.44778(16) 0.0235(7) Uani 1 1 d . . .
C1 C 0.1801(3) 0.9614(3) 0.4045(2) 0.0305(9) Uani 1 1 d . . .
C2 C 0.1076(3) 0.9243(3) 0.4424(2) 0.0256(8) Uani 1 1 d . . .
C3 C 0.0854(3) 0.9239(3) 0.5103(2) 0.0265(8) Uani 1 1 d . . .
H3 H 0.1159 0.9467 0.5464 0.032 Uiso 1 1 calc R . .
C4 C 0.0068(3) 0.8816(3) 0.5109(2) 0.0252(8) Uani 1 1 d . . .
C5 C -0.0585(3) 0.8595(3) 0.5629(2) 0.0275(9) Uani 1 1 d . . .
C6 C 0.3032(4) 1.0481(5) 0.4083(4) 0.0614(18) Uani 1 1 d . . .
H6A H 0.3370 1.0087 0.3820 0.092 Uiso 1 1 calc R . .
H6B H 0.3396 1.0762 0.4406 0.092 Uiso 1 1 calc R . .
H6C H 0.2776 1.0904 0.3794 0.092 Uiso 1 1 calc R . .
C7 C -0.0317(4) 1.0320(4) 0.2399(3) 0.0517(14) Uani 1 1 d . . .
H7A H 0.0187 1.0594 0.2219 0.078 Uiso 1 1 calc R . .
H7B H -0.0752 1.0746 0.2486 0.078 Uiso 1 1 calc R . .
H7C H -0.0533 0.9906 0.2082 0.078 Uiso 1 1 calc R . .
O6 O 0.8374(10) 0.8111(10) 0.7093(9) 0.111(3) Uiso 0.50 1 d PD A 1
C8 C 0.8788(15) 0.7308(12) 0.7183(14) 0.103(7) Uiso 0.50 1 d PD A 1
O6A O 0.8387(10) 0.7077(10) 0.7760(8) 0.111(3) Uiso 0.50 1 d P B 2
C8A C 0.8467(11) 0.7312(10) 0.7021(8) 0.061(4) Uiso 0.50 1 d P B 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O3 Cu1 N2 82.55(13) 10_566 10_566
O3 Cu1 N1 178.74(14) 10_566 .
N2 Cu1 N1 96.40(14) 10_566 .
O3 Cu1 O5 91.89(13) 10_566 .
N2 Cu1 O5 171.19(14) 10_566 .
N1 Cu1 O5 89.24(14) . .
O3 Cu1 O1 104.36(12) 10_566 .
N2 Cu1 O1 96.46(13) 10_566 .
N1 Cu1 O1 75.06(12) . .
O5 Cu1 O1 91.52(12) . .
C1 O1 Cu1 107.0(3) . .
C1 O2 C6 115.6(4) . .
C5 O3 Cu1 115.6(3) . 16_666
C7 O5 Cu1 124.6(3) . .
C7 O5 H5 109(4) . .
Cu1 O5 H5 109(4) . .
N2 N1 C2 107.7(3) . .
N2 N1 Cu1 132.3(3) . .
C2 N1 Cu1 119.9(3) . .
N1 N2 C4 108.8(3) . .
N1 N2 Cu1 138.2(3) . 16_666
C4 N2 Cu1 112.7(3) . 16_666
O1 C1 O2 125.4(4) . .
O1 C1 C2 121.8(4) . .
O2 C1 C2 112.8(4) . .
N1 C2 C3 110.3(4) . .
N1 C2 C1 116.3(4) . .
C3 C2 C1 133.4(4) . .
C4 C3 C2 103.2(4) . .
C4 C3 H3 128.4 . .
C2 C3 H3 128.4 . .
N2 C4 C3 110.1(4) . .
N2 C4 C5 114.3(4) . .
C3 C4 C5 135.6(4) . .
O4 C5 O3 124.5(4) . .
O4 C5 C4 121.3(4) . .
O3 C5 C4 114.3(4) . .
O2 C6 H6A 109.5 . .
O2 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
O2 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
O5 C7 H7A 109.5 . .
O5 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
O5 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O3 1.947(3) 10_566
Cu1 N2 1.953(4) 10_566
Cu1 N1 1.972(4) .
Cu1 O5 1.983(3) .
Cu1 O1 2.436(3) .
O1 C1 1.202(6) .
O2 C1 1.309(5) .
O2 C6 1.450(7) .
O3 C5 1.282(5) .
O3 Cu1 1.947(3) 16_666
O4 C5 1.244(5) .
O5 C7 1.428(6) .
O5 H5 0.857(10) .
N1 N2 1.330(5) .
N1 C2 1.355(5) .
N2 C4 1.351(5) .
N2 Cu1 1.953(4) 16_666
C1 C2 1.471(6) .
C2 C3 1.394(6) .
C3 C4 1.385(6) .
C3 H3 0.9300 .
C4 C5 1.488(6) .
C6 H6A 0.9600 .
C6 H6B 0.9600 .
C6 H6C 0.9600 .
C7 H7A 0.9600 .
C7 H7B 0.9600 .
C7 H7C 0.9600 .
O6 C8 1.412(10) .
O6A C8A 1.52(2) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
O3 Cu1 O1 C1 179.6(3) 10_566 .
N2 Cu1 O1 C1 -96.4(3) 10_566 .
N1 Cu1 O1 C1 -1.5(3) . .
O5 Cu1 O1 C1 87.3(3) . .
O3 Cu1 O5 C7 0.7(4) 10_566 .
N2 Cu1 O5 C7 -49.9(11) 10_566 .
N1 Cu1 O5 C7 -179.8(4) . .
O1 Cu1 O5 C7 105.1(4) . .
O3 Cu1 N1 N2 -121(6) 10_566 .
N2 Cu1 N1 N2 -88.1(4) 10_566 .
O5 Cu1 N1 N2 85.1(4) . .
O1 Cu1 N1 N2 176.9(4) . .
O3 Cu1 N1 C2 64(7) 10_566 .
N2 Cu1 N1 C2 96.2(3) 10_566 .
O5 Cu1 N1 C2 -90.6(3) . .
O1 Cu1 N1 C2 1.2(3) . .
C2 N1 N2 C4 0.2(4) . .
Cu1 N1 N2 C4 -175.8(3) . .
C2 N1 N2 Cu1 173.5(3) . 16_666
Cu1 N1 N2 Cu1 -2.5(6) . 16_666
Cu1 O1 C1 O2 -177.4(4) . .
Cu1 O1 C1 C2 1.6(5) . .
C6 O2 C1 O1 6.4(7) . .
C6 O2 C1 C2 -172.7(5) . .
N2 N1 C2 C3 0.0(5) . .
Cu1 N1 C2 C3 176.7(3) . .
N2 N1 C2 C1 -177.5(3) . .
Cu1 N1 C2 C1 -0.9(5) . .
O1 C1 C2 N1 -0.8(6) . .
O2 C1 C2 N1 178.3(4) . .
O1 C1 C2 C3 -177.6(5) . .
O2 C1 C2 C3 1.5(7) . .
N1 C2 C3 C4 -0.3(5) . .
C1 C2 C3 C4 176.7(5) . .
N1 N2 C4 C3 -0.4(5) . .
Cu1 N2 C4 C3 -175.5(3) 16_666 .
N1 N2 C4 C5 177.5(3) . .
Cu1 N2 C4 C5 2.3(4) 16_666 .
C2 C3 C4 N2 0.4(4) . .
C2 C3 C4 C5 -176.8(5) . .
Cu1 O3 C5 O4 170.6(3) 16_666 .
Cu1 O3 C5 C4 -7.3(5) 16_666 .
N2 C4 C5 O4 -174.7(4) . .
C3 C4 C5 O4 2.4(8) . .
N2 C4 C5 O3 3.3(5) . .
C3 C4 C5 O3 -179.6(4) . .
