#------------------------------------------------------------------------------
#$Date: 2016-03-24 03:00:20 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179608 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/72/4507206.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_4507206
loop_
_publ_author_name
'Di Nicola, Corrado'
'Forlin, Enrico'
'Garau, Federica'
'Gazzano, Massimo'
'Lanza, Arianna'
'Monari, Magda'
'Nestola, Fabrizio'
'Pandolfo, Luciano'
'Pettinari, Claudio'
'Zorzi, Alberto'
'Zorzi, Federico'
_publ_section_title
;
 Coordination Polymers Based on the Trinuclear Triangular Secondary
 Building Unit [Cu3(μ3-OH)(μ-pz)3]2+(pz = pyrazolate) and Succinate
 Anion
;
_journal_issue                   1
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              126
_journal_paper_doi               10.1021/cg3012712
_journal_volume                  13
_journal_year                    2013
_chemical_formula_sum            'C20 H26 Cu N8 O8'
_chemical_formula_weight         570.03
_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            8
_cell_length_a                   22.4290(8)
_cell_length_b                   22.4290(8)
_cell_length_c                   10.2923(7)
_cell_measurement_reflns_used    3000
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.99
_cell_measurement_theta_min      3.37
_cell_volume                     5177.6(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0475
_diffrn_reflns_av_sigmaI/netI    0.0617
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2540
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         3.37
_exptl_absorpt_coefficient_mu    0.903
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.691
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-RED, X-SHAPE (Stoe & Cie)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2360
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.33
_refine_diff_density_max         0.664
_refine_diff_density_min         -0.244
_refine_diff_density_rms         0.042
_refine_ls_extinction_coef       0.00357(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         2540
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0055P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0421
_refine_ls_wR_factor_ref         0.0440
_reflns_number_gt                1502
_reflns_number_total             2540
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg3012712_si_005.cif
_cod_data_source_block           Comp5
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               4507206
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y+1/2, z'
'-y+3/4, x+1/4, z+1/4'
'y+1/4, -x+1/4, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'y+3/4, -x+3/4, z+3/4'
'-x, -y, -z'
'x, y-1/2, -z'
'y-3/4, -x-1/4, -z-1/4'
'-y-1/4, x-1/4, -z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'-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
Cu1 Cu 0.5000 0.0000 0.5000 0.03830(14) Uani 1 2 d S
N1 N 0.52502(7) 0.08625(7) 0.4970(2) 0.0352(4) Uani 1 1 d .
N2 N 0.54694(7) 0.11179(8) 0.39026(19) 0.0393(5) Uani 1 1 d .
H2N H 0.5483 0.0948 0.3154 0.047 Uiso 1 1 calc R
N3 N 0.57918(8) -0.02108(8) 0.57740(19) 0.0357(5) Uani 1 1 d .
N4 N 0.62400(8) -0.04449(7) 0.5082(2) 0.0407(5) Uani 1 1 d .
H4N H 0.6217 -0.0532 0.4270 0.049 Uiso 1 1 calc R
C1 C 0.53137(11) 0.12669(11) 0.5891(2) 0.0520(7) Uani 1 1 d .
H1 H 0.5200 0.1213 0.6752 0.062 Uiso 1 1 calc R
C2 C 0.55709(11) 0.17822(11) 0.5410(3) 0.0542(8) Uani 1 1 d .
H2 H 0.5660 0.2130 0.5861 0.065 Uiso 1 1 calc R
C3 C 0.56644(10) 0.16663(10) 0.4138(3) 0.0489(7) Uani 1 1 d .
H3 H 0.5835 0.1924 0.3535 0.059 Uiso 1 1 calc R
C4 C 0.60107(11) -0.01498(10) 0.6958(2) 0.0505(7) Uani 1 1 d .
H4 H 0.5799 0.0003 0.7660 0.061 Uiso 1 1 calc R
C5 C 0.65963(11) -0.03421(11) 0.7020(3) 0.0584(8) Uani 1 1 d .
H5 H 0.6845 -0.0343 0.7742 0.070 Uiso 1 1 calc R
C6 C 0.67277(10) -0.05266(10) 0.5808(3) 0.0506(7) Uani 1 1 d .
H6 H 0.7090 -0.0682 0.5529 0.061 Uiso 1 1 calc R
O1 O 0.54347(6) -0.02674(6) 0.28999(15) 0.0432(5) Uani 1 1 d .
O3 O 0.66537(7) -0.08133(7) 0.24942(18) 0.0607(5) Uani 1 1 d .
O2 O 0.54417(7) 0.05266(7) 0.16317(15) 0.0524(5) Uani 1 1 d .
O4 O 0.63559(8) -0.17451(9) 0.21667(18) 0.0755(7) Uani 1 1 d .
H4A H 0.6600(11) -0.1847(11) 0.293(3) 0.091 Uiso 1 1 d .
C7 C 0.55399(9) -0.00215(11) 0.1847(2) 0.0370(6) Uani 1 1 d .
C8 C 0.57982(10) -0.03654(10) 0.0719(2) 0.0518(7) Uani 1 1 d .
H8A H 0.5538 -0.0312 -0.0025 0.062 Uiso 1 1 calc R
H8B H 0.6181 -0.0191 0.0499 0.062 Uiso 1 1 calc R
C9 C 0.58852(11) -0.10168(10) 0.0925(2) 0.0600(8) Uani 1 1 d .
H9A H 0.6005 -0.1197 0.0108 0.072 Uiso 1 1 calc R
H9B H 0.5507 -0.1192 0.1174 0.072 Uiso 1 1 calc R
C10 C 0.63439(12) -0.11689(13) 0.1946(2) 0.0518(8) Uani 1 1 d .
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'
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'
Cu Cu 0.3201 1.2651 '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
N3 Cu1 N3 180.00(10) 9_656 .
N3 Cu1 N1 89.18(7) 9_656 9_656
N3 Cu1 N1 90.82(7) . 9_656
N3 Cu1 N1 90.82(7) 9_656 .
N3 Cu1 N1 89.18(7) . .
N1 Cu1 N1 180.00(3) 9_656 .
C1 N1 N2 104.90(17) . .
C1 N1 Cu1 132.79(18) . .
N2 N1 Cu1 121.85(16) . .
C3 N2 N1 111.7(2) . .
C4 N3 N4 104.59(19) . .
C4 N3 Cu1 132.23(18) . .
N4 N3 Cu1 123.14(15) . .
C6 N4 N3 111.8(2) . .
N1 C1 C2 111.2(2) . .
C3 C2 C1 104.5(2) . .
N2 C3 C2 107.7(2) . .
N3 C4 C5 111.3(2) . .
C6 C5 C4 105.1(2) . .
N4 C6 C5 107.2(2) . .
O1 C7 O2 123.4(2) . .
O1 C7 C8 121.2(2) . .
O2 C7 C8 115.3(2) . .
C9 C8 C7 116.2(2) . .
C8 C9 C10 114.2(2) . .
O3 C10 O4 124.2(3) . .
O3 C10 C9 124.9(3) . .
O4 C10 C9 110.9(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N3 2.0030(17) 9_656
Cu1 N3 2.0030(17) .
Cu1 N1 2.0145(16) 9_656
Cu1 N1 2.0145(16) .
N1 C1 1.320(3) .
N1 N2 1.333(2) .
N2 C3 1.328(2) .
N3 C4 1.321(2) .
N3 N4 1.339(2) .
N4 C6 1.337(2) .
C1 C2 1.384(3) .
C2 C3 1.352(3) .
C4 C5 1.384(3) .
C5 C6 1.346(3) .
O1 C7 1.239(2) .
O3 C10 1.199(3) .
O2 C7 1.268(2) .
O4 C10 1.312(3) .
C7 C8 1.509(3) .
C8 C9 1.489(3) .
C9 C10 1.510(3) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N2 H2N O2 0.86 1.83 2.688(2) 173.1 .
N4 H4N O3 0.86 2.17 2.939(3) 149.2 .
N4 H4N O1 0.86 2.33 2.910(2) 125.2 .
O4 H4A O2 0.99(3) 1.56(3) 2.550(2) 176(2) 3_545
