#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:02:40 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179464 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/61/4336177.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_4336177
loop_
_publ_author_name
'Petri Seppälä'
'Enrique Colacio'
'Antonio J. Mota'
'Reijo Sillanpää'
_publ_contact_author_address
;
Department of Chemistry
University of Jyväskylä
P.O.Box 35
FI-40014 University of Jyväskylä
Finland
;
_publ_contact_author_email       resillan@jyu.fi
_publ_contact_author_fax         '+358 14 260 1021'
_publ_contact_author_name        'Sillanpää, Reijo'
_publ_section_title
;
 Structural Diversity due to Amino Alcohol Ligands Leading to Rare
 μ4-Hydroxo-Bridged Tetranuclear and "Bicapped Cubane" Cores in
 Copper(II) Complexes: A Theoretical and Experimental Magnetostructural
 Study
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11096
_journal_page_last               11109
_journal_paper_doi               10.1021/ic401325b
_journal_volume                  52
_journal_year                    2013
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C16 H41 Ag1 Cu4 N8 O17'
_chemical_formula_sum            'C16 H41 Ag Cu4 N8 O17'
_chemical_formula_weight         979.6
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           86
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      86
_symmetry_space_group_name_Hall  '-P 4bc'
_symmetry_space_group_name_H-M   'P 42/n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2013-05-08T11:01:20-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.0938(6)
_cell_length_b                   13.0938(6)
_cell_length_c                   9.4657(3)
_cell_measurement_reflns_used    2122
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      28.283
_cell_measurement_theta_min      0.407
_cell_measurement_wavelength     0.71073
_cell_volume                     1622.87(12)
_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    'DIAMOND (Brandenburg & Putz, 1999)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.518953E-1
_diffrn_orient_matrix_UB_12      0.87386E-2
_diffrn_orient_matrix_UB_13      -0.765597E-1
_diffrn_orient_matrix_UB_21      -0.555601E-1
_diffrn_orient_matrix_UB_22      0.17426E-2
_diffrn_orient_matrix_UB_23      0.724443E-1
_diffrn_orient_matrix_UB_31      0.72552E-2
_diffrn_orient_matrix_UB_32      0.758504E-1
_diffrn_orient_matrix_UB_33      0.71559E-2
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_unetI/netI     0.0336
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            9956
_diffrn_reflns_theta_full        25.98
_diffrn_reflns_theta_max         25.98
_diffrn_reflns_theta_min         2.15
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    3.253
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5282
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Bruker (2001). SADABS-2008/1. Bruker AXS Inc., Madison, Wisconsin, USA.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.005
_exptl_crystal_description       plate
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.755
_refine_diff_density_min         -0.526
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     111
_refine_ls_number_reflns         1593
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0685
_refine_ls_R_factor_gt           0.0521
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0003P)²+8.2220P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.095
_refine_ls_wR_factor_ref         0.1023
_reflns_number_gt                1314
_reflns_number_total             1593
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ic401325b_si_002_2.cif
_cod_data_source_block           import_Complex1
_cod_original_sg_symbol_H-M      'P 42/n'
_cod_database_code               4336177
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x+1/2, z+1/2'
'-x+1/2, -y+1/2, z'
'y+1/2, -x, z+1/2'
'-x, -y, -z'
'y, -x-1/2, -z-1/2'
'x-1/2, y-1/2, -z'
'-y-1/2, x, -z-1/2'
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
C1 C 1.0035(7) 0.8830(8) 0.1576(13) 0.078(3) Uani 1 1 d .
H1A H 1.0353 0.9485 0.186 0.094 Uiso 1 1 calc R
H1B H 0.9771 0.8904 0.0602 0.094 Uiso 1 1 calc R
C2 C 1.0862(8) 0.7928(9) 0.1642(12) 0.086(3) Uani 1 1 d .
H2A H 1.1364 0.8006 0.0868 0.103 Uiso 1 1 calc R
H2B H 1.1233 0.795 0.2553 0.103 Uiso 1 1 calc R
C3 C 1.0039(8) 0.6786(10) 0.0020(9) 0.087(4) Uani 1 1 d .
H3A H 1.0661 0.6733 -0.0553 0.13 Uiso 1 1 calc R
H3B H 0.9628 0.7363 -0.0314 0.13 Uiso 1 1 calc R
H3C H 0.9644 0.6154 -0.0067 0.13 Uiso 1 1 calc R
C4 C 1.0978(9) 0.6138(10) 0.1957(11) 0.102(4) Uani 1 1 d .
H4A H 1.1134 0.6225 0.2962 0.153 Uiso 1 1 calc R
H4B H 1.1614 0.6157 0.141 0.153 Uiso 1 1 calc R
H4C H 1.0639 0.5479 0.1812 0.153 Uiso 1 1 calc R
Ag1 Ag 0.75 0.75 0.75 0.0768(5) Uani 1 4 d S
Cu1 Cu 0.90439(7) 0.71403(7) 0.26386(8) 0.0429(2) Uani 1 1 d .
N1 N 1.0316(5) 0.6947(5) 0.1497(6) 0.0447(15) Uani 1 1 d .
N2 N 0.9409(5) 0.7155(5) 0.5704(7) 0.0503(16) Uani 1 1 d .
O1 O 0.9239(3) 0.8582(4) 0.2500(6) 0.0509(13) Uani 1 1 d .
O2 O 0.75 0.75 0.2130(12) 0.036(4) Uani 0.5 2 d SPD
O3 O 0.8589(6) 0.7255(6) 0.5109(8) 0.101(3) Uani 1 1 d .
O4 O 0.9480(5) 0.7187(5) 0.6972(5) 0.0640(17) Uani 1 1 d .
O5 O 1.0173(6) 0.7012(5) 0.4952(7) 0.087(2) Uani 1 1 d .
H2O H 0.75 0.75 0.124(3) 0.05 Uiso 0.5 2 d SPD
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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag -0.8971 1.1015 '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 0.006 '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
O1 C1 C2 107.9(8) . .
O1 C1 H1A 110.1 . .
C2 C1 H1A 110.1 . .
O1 C1 H1B 110.1 . .
C2 C1 H1B 110.1 . .
H1A C1 H1B 108.4 . .
N1 C2 C1 108.1(8) . .
N1 C2 H2A 110.1 . .
C1 C2 H2A 110.1 . .
N1 C2 H2B 110.1 . .
C1 C2 H2B 110.1 . .
H2A C2 H2B 108.4 . .
N1 C3 H3A 109.5 . .
N1 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
N1 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
N1 C4 H4A 109.5 . .
N1 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
N1 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
O4 Ag1 O3 46.45(17) . .
O1 Cu1 O1 166.64(19) 6_576 .
O1 Cu1 N1 96.1(2) 6_576 .
O1 Cu1 N1 88.7(2) . .
O1 Cu1 O2 85.07(16) 6_576 6_576
O1 Cu1 O2 85.05(14) . 6_576
N1 Cu1 O2 153.0(4) . 6_576
O1 Cu1 O2 83.87(15) 6_576 .
O1 Cu1 O2 83.85(14) . .
N1 Cu1 O2 134.1(4) . .
O2 Cu1 O2 19.1(6) 6_576 .
O1 Cu1 O3 92.7(3) 6_576 .
O1 Cu1 O3 92.2(3) . .
N1 Cu1 O3 137.3(3) . .
O2 Cu1 O3 69.3(4) 6_576 .
O2 Cu1 O3 88.3(4) . .
O1 Cu1 Cu1 39.50(15) 6_576 6_576
O1 Cu1 Cu1 128.84(14) . 6_576
N1 Cu1 Cu1 126.11(18) . 6_576
O2 Cu1 Cu1 46.28(7) 6_576 6_576
O2 Cu1 Cu1 45.07(3) . 6_576
O3 Cu1 Cu1 84.85(19) . 6_576
O1 Cu1 Cu1 128.86(15) 6_576 8_756
O1 Cu1 Cu1 39.48(14) . 8_756
N1 Cu1 Cu1 119.78(19) . 8_756
O2 Cu1 Cu1 46.28(7) 6_576 8_756
O2 Cu1 Cu1 45.07(3) . 8_756
O3 Cu1 Cu1 84.50(18) . 8_756
Cu1 Cu1 Cu1 89.546(6) 6_576 8_756
C4 N1 C3 109.5(8) . .
C4 N1 C2 108.8(8) . .
C3 N1 C2 109.6(8) . .
C4 N1 Cu1 115.6(6) . .
C3 N1 Cu1 109.2(5) . .
C2 N1 Cu1 104.1(5) . .
O4 N2 O3 121.6(8) . .
O4 N2 O5 120.9(8) . .
O3 N2 O5 117.4(8) . .
C1 O1 Cu1 126.1(6) . 8_756
C1 O1 Cu1 111.8(5) . .
Cu1 O1 Cu1 101.0(2) 8_756 .
O2 O2 H2O 180.000(14) 6_576 .
O2 O2 Cu1 84.0(3) 6_576 8_756
H2O O2 Cu1 96.0(3) . 8_756
O2 O2 Cu1 84.0(3) 6_576 6_576
H2O O2 Cu1 96.0(3) . 6_576
Cu1 O2 Cu1 168.0(6) 8_756 6_576
O2 O2 Cu1 76.9(3) 6_576 .
H2O O2 Cu1 103.1(3) . .
Cu1 O2 Cu1 88.64(10) 8_756 .
Cu1 O2 Cu1 88.64(10) 6_576 .
O2 O2 Cu1 76.9(3) 6_576 3_665
H2O O2 Cu1 103.1(3) . 3_665
Cu1 O2 Cu1 88.64(10) 8_756 3_665
Cu1 O2 Cu1 88.64(10) 6_576 3_665
Cu1 O2 Cu1 153.9(6) . 3_665
O2 O2 H2O 180.000(14) 6_576 .
H2O O2 H2O 0.000(7) . .
Cu1 O2 H2O 96.0(3) 8_756 .
Cu1 O2 H2O 96.0(3) 6_576 .
Cu1 O2 H2O 103.1(3) . .
Cu1 O2 H2O 103.1(3) 3_665 .
N2 O3 Cu1 102.9(6) . .
N2 O3 Ag1 95.2(5) . .
Cu1 O3 Ag1 161.9(3) . .
N2 O4 Ag1 96.7(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O1 1.399(10) .
C1 C2 1.604(14) .
C1 H1A 0.99 .
C1 H1B 0.99 .
C2 N1 1.476(12) .
C2 H2A 0.99 .
C2 H2B 0.99 .
C3 N1 1.460(10) .
C3 H3A 0.98 .
C3 H3B 0.98 .
C3 H3C 0.98 .
C4 N1 1.437(10) .
C4 H4A 0.98 .
C4 H4B 0.98 .
C4 H4C 0.98 .
Ag1 O4 2.672(6) .
Ag1 O3 2.694(9) .
Cu1 O1 1.909(5) 6_576
Cu1 O1 1.910(5) .
Cu1 N1 2.002(6) .
Cu1 O2 2.0873(15) 6_576
Cu1 O2 2.131(3) .
Cu1 O3 2.418(8) .
Cu1 Cu1 2.9472(12) 6_576
Cu1 Cu1 2.9472(12) 8_756
N2 O4 1.204(7) .
N2 O3 1.220(9) .
N2 O5 1.242(8) .
O1 Cu1 1.909(5) 8_756
O2 O2 0.70(2) 6_576
O2 H2O 0.85(2) .
O2 Cu1 2.0873(15) 8_756
O2 Cu1 2.0873(15) 6_576
O2 Cu1 2.131(3) 3_665
O2 H2O 0.85(2) .
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
O2 H2O O3 0.85(2) 1.939(17) 2.574(12) 131.1(6) 6_576
O2 H2O O3 0.85(2) 1.939(17) 2.574(12) 131.1(6) 8_756
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
O1 C1 C2 N1 48.4(12) . .
C1 C2 N1 C4 -163.4(8) . .
C1 C2 N1 C3 77.0(10) . .
C1 C2 N1 Cu1 -39.7(9) . .
O1 Cu1 N1 C4 -53.6(8) 6_576 .
O1 Cu1 N1 C4 138.9(8) . .
O2 Cu1 N1 C4 -144.8(7) 6_576 .
O2 Cu1 N1 C4 -141.0(7) . .
O3 Cu1 N1 C4 47.1(9) . .
Cu1 Cu1 N1 C4 -81.7(7) 6_576 .
Cu1 Cu1 N1 C4 164.4(7) 8_756 .
O1 Cu1 N1 C3 70.3(7) 6_576 .
O1 Cu1 N1 C3 -97.2(6) . .
O2 Cu1 N1 C3 -20.9(9) 6_576 .
O2 Cu1 N1 C3 -17.1(7) . .
O3 Cu1 N1 C3 171.0(6) . .
Cu1 Cu1 N1 C3 42.2(7) 6_576 .
Cu1 Cu1 N1 C3 -71.7(7) 8_756 .
O1 Cu1 N1 C2 -172.8(6) 6_576 .
O1 Cu1 N1 C2 19.7(6) . .
O2 Cu1 N1 C2 96.0(7) 6_576 .
O2 Cu1 N1 C2 99.8(6) . .
O3 Cu1 N1 C2 -72.0(7) . .
Cu1 Cu1 N1 C2 159.1(5) 6_576 .
Cu1 Cu1 N1 C2 45.2(6) 8_756 .
C2 C1 O1 Cu1 -154.4(6) . 8_756
C2 C1 O1 Cu1 -31.2(10) . .
O1 Cu1 O1 C1 -103.7(9) 6_576 .
N1 Cu1 O1 C1 7.7(6) . .
O2 Cu1 O1 C1 -146.1(7) 6_576 .
O2 Cu1 O1 C1 -126.9(7) . .
O3 Cu1 O1 C1 145.0(6) . .
Cu1 Cu1 O1 C1 -129.9(6) 6_576 .
Cu1 Cu1 O1 C1 -136.4(7) 8_756 .
O1 Cu1 O1 Cu1 32.8(5) 6_576 8_756
N1 Cu1 O1 Cu1 144.1(3) . 8_756
O2 Cu1 O1 Cu1 -9.6(4) 6_576 8_756
O2 Cu1 O1 Cu1 9.5(4) . 8_756
O3 Cu1 O1 Cu1 -78.6(3) . 8_756
Cu1 Cu1 O1 Cu1 6.5(4) 6_576 8_756
O1 Cu1 O2 O2 92.63(18) 6_576 6_576
O1 Cu1 O2 O2 -92.64(18) . 6_576
N1 Cu1 O2 O2 -174.7(3) . 6_576
O3 Cu1 O2 O2 -0.25(19) . 6_576
Cu1 Cu1 O2 O2 84.1(3) 6_576 6_576
Cu1 Cu1 O2 O2 -84.1(3) 8_756 6_576
O1 Cu1 O2 H2O -87.37(18) 6_576 .
O1 Cu1 O2 H2O 87.36(18) . .
N1 Cu1 O2 H2O 5.3(3) . .
O2 Cu1 O2 H2O 180.000(3) 6_576 .
O3 Cu1 O2 H2O 179.75(19) . .
Cu1 Cu1 O2 H2O -95.9(3) 6_576 .
Cu1 Cu1 O2 H2O 95.9(3) 8_756 .
O1 Cu1 O2 Cu1 176.8(4) 6_576 8_756
O1 Cu1 O2 Cu1 -8.5(3) . 8_756
N1 Cu1 O2 Cu1 -90.6(4) . 8_756
O2 Cu1 O2 Cu1 84.1(3) 6_576 8_756
O3 Cu1 O2 Cu1 83.9(4) . 8_756
Cu1 Cu1 O2 Cu1 168.3(6) 6_576 8_756
O1 Cu1 O2 Cu1 8.5(3) 6_576 6_576
O1 Cu1 O2 Cu1 -176.8(4) . 6_576
N1 Cu1 O2 Cu1 101.1(4) . 6_576
O2 Cu1 O2 Cu1 -84.1(3) 6_576 6_576
O3 Cu1 O2 Cu1 -84.4(4) . 6_576
Cu1 Cu1 O2 Cu1 -168.3(6) 8_756 6_576
O1 Cu1 O2 Cu1 92.63(18) 6_576 3_665
O1 Cu1 O2 Cu1 -92.64(18) . 3_665
N1 Cu1 O2 Cu1 -174.7(3) . 3_665
O2 Cu1 O2 Cu1 0 6_576 3_665
O3 Cu1 O2 Cu1 -0.25(19) . 3_665
Cu1 Cu1 O2 Cu1 84.1(3) 6_576 3_665
Cu1 Cu1 O2 Cu1 -84.1(3) 8_756 3_665
O4 N2 O3 Cu1 179.0(6) . .
O5 N2 O3 Cu1 -1.6(9) . .
O4 N2 O3 Ag1 0.3(9) . .
O5 N2 O3 Ag1 179.7(6) . .
O1 Cu1 O3 N2 101.8(6) 6_576 .
O1 Cu1 O3 N2 -90.6(6) . .
N1 Cu1 O3 N2 -0.2(8) . .
O2 Cu1 O3 N2 -174.5(6) 6_576 .
O2 Cu1 O3 N2 -174.4(6) . .
Cu1 Cu1 O3 N2 140.6(6) 6_576 .
Cu1 Cu1 O3 N2 -129.4(6) 8_756 .
O1 Cu1 O3 Ag1 -82.3(12) 6_576 .
O1 Cu1 O3 Ag1 85.2(12) . .
N1 Cu1 O3 Ag1 175.6(10) . .
O2 Cu1 O3 Ag1 1.4(11) 6_576 .
O2 Cu1 O3 Ag1 1.5(12) . .
Cu1 Cu1 O3 Ag1 -43.6(11) 6_576 .
Cu1 Cu1 O3 Ag1 46.5(11) 8_756 .
O4 Ag1 O3 N2 -0.1(5) . .
O4 Ag1 O3 Cu1 -176.1(13) . .
O3 N2 O4 Ag1 -0.3(9) . .
O5 N2 O4 Ag1 -179.7(6) . .
O3 Ag1 O4 N2 0.1(5) . .
