#------------------------------------------------------------------------------
#$Date: 2016-03-21 18:43:46 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178821 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/75/4107514.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_4107514
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            'C8 H4 Cu O4.11'
_chemical_formula_weight         229.44
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           176
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_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                120.00
_cell_formula_units_Z            6
_cell_length_a                   9.1056(3)
_cell_length_b                   9.1056(3)
_cell_length_c                   15.9550(12)
_cell_measurement_reflns_used    4905
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.46
_cell_measurement_theta_min      2.55
_cell_volume                     1145.63(10)
_computing_cell_refinement       'SAINT 5 (Bruker-AXS, 2003)'
_computing_data_collection       'SMART 5 (Bruker-AXS, 2003)'
_computing_data_reduction        'SAINT 5 (Bruker-AXS, 2003)'
_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_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0311
_diffrn_reflns_av_sigmaI/netI    0.0110
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            22913
_diffrn_reflns_theta_full        29.55
_diffrn_reflns_theta_max         29.55
_diffrn_reflns_theta_min         2.55
_exptl_absorpt_coefficient_mu    2.832
_exptl_absorpt_correction_T_max  0.7649
_exptl_absorpt_correction_T_min  0.6760
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.995
_exptl_crystal_description       plate
_exptl_crystal_F_000             683
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.578
_refine_diff_density_min         -1.128
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     66
_refine_ls_number_reflns         1118
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0235
_refine_ls_R_factor_gt           0.0217
_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)+(0.0388P)²+0.4063P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0621
_refine_ls_wR_factor_ref         0.0637
_reflns_number_gt                1042
_reflns_number_total             1118
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja709991u-file003.cif
_cod_data_source_block           05251
_cod_database_code               4107514
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -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
Cu1 Cu 0.5000 0.5000 0.0000 0.00820(10) Uani 1 2 d S
O1 O 0.63608(10) 0.57899(10) 0.10016(5) 0.01126(18) Uani 1 1 d .
O2 O 0.42587(11) 0.26457(10) 0.02613(5) 0.01294(19) Uani 1 1 d .
C1 C 0.78264(14) 0.59610(13) 0.09502(7) 0.0098(2) Uani 1 1 d .
C2 C 0.88376(14) 0.64352(14) 0.17413(7) 0.0098(2) Uani 1 1 d .
C3 C 1.06117(14) 0.72496(14) 0.17406(7) 0.0117(2) Uani 1 1 d .
H3 H 1.1216 0.7523 0.1226 0.014 Uiso 1 1 calc R
C4 C 1.1484(2) 0.7656(2) 0.2500 0.0124(3) Uani 1 2 d S
H4 H 1.2687 0.8216 0.2500 0.015 Uiso 1 2 calc SR
C5 C 0.7963(2) 0.6049(2) 0.2500 0.0099(3) Uani 1 2 d S
H5 H 0.6761 0.5519 0.2500 0.012 Uiso 1 2 calc SR
O3 O 0.0000 0.0000 0.0000 0.061(4) Uani 0.33 6 d SP
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.00977(13) 0.00955(13) 0.00593(16) 0.00022(6) -0.00080(6) 0.00533(9)
O1 0.0115(4) 0.0143(4) 0.0090(4) -0.0001(3) -0.0008(3) 0.0072(3)
O2 0.0187(4) 0.0122(4) 0.0081(4) 0.0004(3) -0.0006(3) 0.0079(3)
C1 0.0112(5) 0.0090(5) 0.0085(5) 0.0010(4) 0.0000(4) 0.0045(4)
C2 0.0115(5) 0.0105(5) 0.0079(5) -0.0004(4) -0.0012(4) 0.0058(4)
C3 0.0107(5) 0.0118(5) 0.0113(5) 0.0004(4) 0.0016(4) 0.0047(4)
C4 0.0086(7) 0.0125(7) 0.0134(7) 0.000 0.000 0.0032(6)
C5 0.0095(7) 0.0100(7) 0.0103(7) 0.000 0.000 0.0050(6)
O3 0.054(6) 0.054(6) 0.075(12) 0.000 0.000 0.027(3)
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
O1 Cu1 O1 180.00(3) 7_665 .
O1 Cu1 O2 87.84(3) 7_665 .
O1 Cu1 O2 92.16(3) . .
O1 Cu1 O2 92.16(3) 7_665 7_665
O1 Cu1 O2 87.84(3) . 7_665
O2 Cu1 O2 180.00(5) . 7_665
C1 O1 Cu1 115.69(7) . .
C1 O2 Cu1 132.36(8) 2_655 .
O1 C1 O2 121.25(10) . 3_665
O1 C1 C2 116.12(10) . .
O2 C1 C2 122.63(10) 3_665 .
C5 C2 C3 119.78(11) . .
C5 C2 C1 117.97(10) . .
C3 C2 C1 122.25(10) . .
C4 C3 C2 119.55(11) . .
C3 C4 C3 120.81(15) . 10_556
C2 C5 C2 120.53(14) 10_556 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O1 1.9275(8) 7_665
Cu1 O1 1.9275(8) .
Cu1 O2 1.9437(8) .
Cu1 O2 1.9437(8) 7_665
O1 C1 1.2665(14) .
O2 C1 1.2692(14) 2_655
C1 O2 1.2692(14) 3_665
C1 C2 1.4932(15) .
C2 C5 1.3940(13) .
C2 C3 1.4006(16) .
C3 C4 1.3934(14) .
C4 C3 1.3934(14) 10_556
C5 C2 1.3940(13) 10_556
