#------------------------------------------------------------------------------
#$Date: 2016-03-21 17:43:46 +0100 (lun 21 de mar de 2016) $
#$Revision: 178821 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/75/4107515.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_4107515
loop_
_publ_author_name
'Emily A. Nytko'
'Joel S. Helton'
'Peter Müller'
'Daniel G. Nocera'
_publ_section_title
;
 A Structurally Perfect S=1/2 Metal-Organic Hybrid Kagomé
 Antiferromagnet
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2922
_journal_page_last               2923
_journal_paper_doi               10.1021/ja709991u
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C32 H24 Cu6 O26'
_chemical_formula_weight         1205.75
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                104.0140(10)
_cell_angle_beta                 99.4120(10)
_cell_angle_gamma                98.2080(10)
_cell_formula_units_Z            1
_cell_length_a                   7.0738(6)
_cell_length_b                   10.8611(8)
_cell_length_c                   12.0790(9)
_cell_measurement_reflns_used    7078
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.06
_cell_measurement_theta_min      2.26
_cell_volume                     872.01(12)
_computing_cell_refinement       'SAINT 7 (Bruker-AXS, 2005)'
_computing_data_collection       'SMART 5 (Bruker-AXS, 2003)'
_computing_data_reduction        'SAINT 7 (Bruker-AXS, 2005)'
_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      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       'omega and phi scans'
_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  0.0450
_diffrn_reflns_av_sigmaI/netI    0.0452
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18271
_diffrn_reflns_theta_full        29.13
_diffrn_reflns_theta_max         29.13
_diffrn_reflns_theta_min         1.97
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.705
_exptl_absorpt_correction_T_max  0.9296
_exptl_absorpt_correction_T_min  0.5245
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2005)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.296
_exptl_crystal_description       plate
_exptl_crystal_F_000             598
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.689
_refine_diff_density_min         -0.540
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         4692
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0333
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0359P)²+0.0909P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0699
_refine_ls_wR_factor_ref         0.0768
_reflns_number_gt                3645
_reflns_number_total             4692
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja709991u-file004.cif
_cod_data_source_block           06218
_cod_database_code               4107515
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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 0.64719(5) 0.36101(3) -0.00800(3) 0.01047(8) Uani 1 1 d .
Cu2 Cu 0.85890(5) 0.62256(3) 0.00503(3) 0.01032(8) Uani 1 1 d .
Cu3 Cu 0.38423(5) 0.09955(3) 0.23048(3) 0.01314(9) Uani 1 1 d .
O1 O 0.8901(3) 0.78581(18) 0.11211(16) 0.0124(4) Uani 1 1 d .
O2 O 0.8597(3) 0.92656(18) 0.27119(17) 0.0134(4) Uani 1 1 d .
O3 O 0.4939(3) 0.30194(18) 0.09067(16) 0.0136(4) Uani 1 1 d .
O4 O 0.4416(3) 0.28873(17) 0.26293(17) 0.0122(4) Uani 1 1 d .
O5 O 1.0652(3) 0.69665(18) -0.26499(17) 0.0124(4) Uani 1 1 d .
O6 O 1.0140(3) 0.67970(18) -0.09359(17) 0.0134(4) Uani 1 1 d .
O7 O 0.6048(3) 0.19933(18) -0.11913(16) 0.0127(4) Uani 1 1 d .
O8 O 0.6403(3) 0.06052(18) -0.27761(17) 0.0146(4) Uani 1 1 d .
O9 O 0.2253(4) 0.0379(2) 0.0463(2) 0.0370(7) Uani 1 1 d D
H9A H 0.110(3) 0.020(4) 0.047(4) 0.056 Uiso 1 1 d D
H9B H 0.235(6) 0.088(3) 0.006(3) 0.056 Uiso 1 1 d D
O10 O 0.1550(3) 0.12097(19) 0.29822(19) 0.0154(4) Uani 1 1 d D
H10A H 0.097(4) 0.175(2) 0.278(3) 0.023 Uiso 1 1 d D
H10B H 0.066(4) 0.057(2) 0.286(3) 0.023 Uiso 1 1 d D
O11 O 0.6415(3) 0.0882(2) 0.1946(3) 0.0316(6) Uani 1 1 d D
H11A H 0.721(5) 0.156(2) 0.212(4) 0.047 Uiso 1 1 d D
H11B H 0.707(5) 0.034(3) 0.210(4) 0.047 Uiso 1 1 d D
O13 O 0.6970(3) 0.53699(17) 0.08802(16) 0.0110(4) Uani 1 1 d .
O12 O 0.8049(3) 0.44690(17) -0.09303(16) 0.0103(4) Uani 1 1 d .
C11 C 0.7636(4) 0.7083(3) 0.2651(2) 0.0101(5) Uani 1 1 d .
C12 C 0.6904(4) 0.5777(3) 0.2024(2) 0.0096(5) Uani 1 1 d .
C13 C 0.6079(4) 0.4898(2) 0.2589(2) 0.0089(5) Uani 1 1 d .
C14 C 0.6121(4) 0.5343(3) 0.3788(2) 0.0108(5) Uani 1 1 d .
H14 H 0.5596 0.4756 0.4178 0.013 Uiso 1 1 calc R
C15 C 0.6894(4) 0.6599(3) 0.4412(2) 0.0128(6) Uani 1 1 d .
H15 H 0.6939 0.6868 0.5226 0.015 Uiso 1 1 calc R
C16 C 0.7610(4) 0.7471(3) 0.3842(2) 0.0119(5) Uani 1 1 d .
H16 H 0.8092 0.8349 0.4266 0.014 Uiso 1 1 calc R
C21 C 0.8860(4) 0.4960(3) -0.2649(2) 0.0100(5) Uani 1 1 d .
C22 C 0.8048(4) 0.4083(3) -0.2084(2) 0.0092(5) Uani 1 1 d .
C23 C 0.7295(4) 0.2780(3) -0.2715(2) 0.0113(5) Uani 1 1 d .
C24 C 0.7297(4) 0.2400(3) -0.3909(2) 0.0117(5) Uani 1 1 d .
H24 H 0.6809 0.1523 -0.4336 0.014 Uiso 1 1 calc R
C25 C 0.7996(4) 0.3275(3) -0.4483(2) 0.0132(6) Uani 1 1 d .
H25 H 0.7930 0.3012 -0.5301 0.016 Uiso 1 1 calc R
C26 C 0.8790(4) 0.4537(3) -0.3849(2) 0.0117(5) Uani 1 1 d .
H26 H 0.9300 0.5132 -0.4236 0.014 Uiso 1 1 calc R
C110 C 0.8423(4) 0.8119(3) 0.2124(2) 0.0114(5) Uani 1 1 d .
C130 C 0.5117(4) 0.3530(3) 0.2000(2) 0.0109(5) Uani 1 1 d .
C210 C 0.9923(4) 0.6319(3) -0.2047(2) 0.0109(5) Uani 1 1 d .
C230 C 0.6541(4) 0.1750(3) -0.2171(2) 0.0113(5) 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'
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
O7 Cu1 O3 95.27(8) . .
O7 Cu1 O12 93.37(8) . .
O3 Cu1 O12 171.28(8) . .
O7 Cu1 O13 171.89(8) . .
O3 Cu1 O13 92.07(8) . .
O12 Cu1 O13 79.23(8) . .
O7 Cu1 Cu2 133.08(6) . .
O3 Cu1 Cu2 131.56(6) . .
O12 Cu1 Cu2 39.75(5) . .
O13 Cu1 Cu2 39.49(5) . .
O1 Cu2 O6 95.90(8) . .
O1 Cu2 O13 93.45(8) . .
O6 Cu2 O13 170.65(8) . .
O1 Cu2 O12 172.63(8) . .
O6 Cu2 O12 91.46(8) . .
O13 Cu2 O12 79.19(8) . .
O1 Cu2 Cu1 133.06(6) . .
O6 Cu2 Cu1 131.03(6) . .
O13 Cu2 Cu1 39.62(5) . .
O12 Cu2 Cu1 39.58(5) . .
O8 Cu3 O10 83.46(8) 2_655 .
O8 Cu3 O11 93.71(9) 2_655 .
O10 Cu3 O11 168.69(11) . .
O8 Cu3 O4 152.98(8) 2_655 .
O10 Cu3 O4 86.66(8) . .
O11 Cu3 O4 91.08(9) . .
O8 Cu3 O9 103.46(9) 2_655 .
O10 Cu3 O9 96.01(10) . .
O11 Cu3 O9 95.29(12) . .
O4 Cu3 O9 102.55(9) . .
C110 O1 Cu2 127.92(17) . .
C130 O3 Cu1 126.16(17) . .
C130 O4 Cu3 126.70(17) . .
C210 O6 Cu2 126.77(17) . .
C230 O7 Cu1 127.52(17) . .
C230 O8 Cu3 129.34(18) . 2_655
C12 O13 Cu2 126.82(16) . .
C12 O13 Cu1 127.37(16) . .
Cu2 O13 Cu1 100.89(8) . .
C22 O12 Cu1 127.00(16) . .
C22 O12 Cu2 127.04(16) . .
Cu1 O12 Cu2 100.67(8) . .
C16 C11 C12 119.0(2) . .
C16 C11 C110 116.5(2) . .
C12 C11 C110 124.5(2) . .
O13 C12 C11 120.1(2) . .
O13 C12 C13 120.1(2) . .
C11 C12 C13 119.8(2) . .
C14 C13 C12 118.3(2) . .
C14 C13 C130 116.9(2) . .
C12 C13 C130 124.8(2) . .
C15 C14 C13 122.1(2) . .
C14 C15 C16 119.3(3) . .
C15 C16 C11 121.3(2) . .
C26 C21 C22 119.0(2) . .
C26 C21 C210 116.2(2) . .
C22 C21 C210 124.8(2) . .
O12 C22 C21 120.5(2) . .
O12 C22 C23 119.7(2) . .
C21 C22 C23 119.8(2) . .
C24 C23 C22 118.9(2) . .
C24 C23 C230 117.4(2) . .
C22 C23 C230 123.7(2) . .
C25 C24 C23 121.5(3) . .
C26 C25 C24 119.0(3) . .
C25 C26 C21 121.7(2) . .
O2 C110 O1 120.9(2) . .
O2 C110 C11 116.7(2) . .
O1 C110 C11 122.5(2) . .
O4 C130 O3 120.5(2) . .
O4 C130 C13 116.6(2) . .
O3 C130 C13 122.9(2) . .
O5 C210 O6 120.6(2) . .
O5 C210 C21 117.8(2) . .
O6 C210 C21 121.6(2) . .
O8 C230 O7 121.6(2) . .
O8 C230 C23 114.9(2) . .
O7 C230 C23 123.5(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O7 1.8846(19) .
Cu1 O3 1.8980(19) .
Cu1 O12 1.9267(18) .
Cu1 O13 1.9295(18) .
Cu1 Cu2 2.9714(5) .
Cu2 O1 1.8840(19) .
Cu2 O6 1.8969(19) .
Cu2 O13 1.9244(18) .
Cu2 O12 1.9334(18) .
Cu3 O8 1.9500(19) 2_655
Cu3 O10 1.950(2) .
Cu3 O11 1.952(2) .
Cu3 O4 1.9647(18) .
Cu3 O9 2.216(3) .
O1 C110 1.288(3) .
O2 C110 1.252(3) .
O3 C130 1.280(3) .
O4 C130 1.262(3) .
O5 C210 1.248(3) .
O6 C210 1.291(3) .
O7 C230 1.266(3) .
O8 C230 1.262(3) .
O8 Cu3 1.9500(19) 2_655
O13 C12 1.355(3) .
O12 C22 1.354(3) .
C11 C16 1.401(4) .
C11 C12 1.412(4) .
C11 C110 1.505(4) .
C12 C13 1.416(3) .
C13 C14 1.405(4) .
C13 C130 1.490(4) .
C14 C15 1.371(4) .
C15 C16 1.386(4) .
C21 C26 1.400(4) .
C21 C22 1.411(4) .
C21 C210 1.503(4) .
C22 C23 1.413(4) .
C23 C24 1.401(4) .
C23 C230 1.505(4) .
C24 C25 1.388(4) .
C25 C26 1.383(4) .
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
O9 H9A O9 0.809(18) 2.38(3) 3.119(6) 153(4) 2
O9 H9B O1 0.820(18) 2.36(3) 3.115(3) 154(4) 2_665
O9 H9B O3 0.820(18) 2.61(4) 3.080(3) 118(3) .
O10 H10A O5 0.821(17) 1.946(19) 2.752(3) 166(3) 2_665
O10 H10B O2 0.837(17) 1.833(18) 2.667(3) 174(3) 1_445
O11 H11A O5 0.823(18) 1.93(2) 2.751(3) 171(4) 2_765
O11 H11B O2 0.836(18) 1.89(2) 2.723(3) 171(4) 1_545
