#------------------------------------------------------------------------------
#$Date: 2016-03-23 14:43:37 +0100 (Wed 23 de Mar de 2016) $
#$Revision: 179344 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/41/4324143.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_4324143
loop_
_publ_author_name
'Wei-Xiong Zhang'
'Wei Xue'
'Xiao-Ming Chen'
_publ_section_title
;
 Flexible Mixed-Spin Kagomé Coordination Polymers with Reversible
 Magnetism Triggered by Dehydration and Rehydration
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              309
_journal_page_last               316
_journal_paper_doi               10.1021/ic101948q
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C8 H8 Cu2 Fe N6 O12'
_chemical_formula_weight         563.13
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_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                 104.213(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.3363(14)
_cell_length_b                   12.020(2)
_cell_length_c                   8.6697(16)
_cell_measurement_reflns_used    935
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.564
_cell_measurement_theta_min      3.328
_cell_volume                     741.1(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker Apex CCd'
_diffrn_measurement_method       'ω scan'
_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  0.0183
_diffrn_reflns_av_sigmaI/netI    0.0288
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            1712
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         3.39
_exptl_absorpt_coefficient_mu    3.901
_exptl_absorpt_correction_T_max  0.8288
_exptl_absorpt_correction_T_min  0.7719
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_diffrn    2.524
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             556
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.462
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     73
_refine_ls_number_reflns         765
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0262
_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)+(0.0385P)²+0.7250P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0687
_refine_ls_wR_factor_ref         0.0715
_reflns_number_gt                705
_reflns_number_total             765
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101948q_si_002.cif
_cod_data_source_block           1
_cod_database_code               4324143
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.0000 0.0000 0.5000 0.0157(2) Uani 1 4 d S . .
Cu1 Cu 0.2500 0.2500 0.0000 0.01782(19) Uani 1 2 d S . .
C1 C 0.1174(4) 0.1489(2) 0.2383(3) 0.0161(5) Uani 1 1 d . . .
C2 C 0.1875(3) 0.0575(2) 0.1537(3) 0.0150(5) Uani 1 1 d . . .
N1 N 0.2533(3) 0.08836(19) 0.0273(3) 0.0157(5) Uani 1 1 d . . .
N2 N 0.2927(4) 0.0000 -0.0488(4) 0.0159(6) Uani 1 2 d S . .
O1W O -0.2861(4) 0.0000 0.3794(3) 0.0258(6) Uani 1 2 d S . .
H1WB H -0.3348 0.0591 0.4053 0.031 Uiso 0.50 1 d PR . .
H1WA H -0.3045 0.0000 0.2787 0.031 Uiso 1 2 d SR . .
O1 O 0.1235(3) 0.24482(14) 0.1764(3) 0.0223(5) Uani 1 1 d . . .
O2 O 0.0498(3) 0.13126(15) 0.3537(2) 0.0226(4) Uani 1 1 d . . .
O2W O -0.5000 -0.1491(3) 0.5000 0.0534(11) Uani 1 2 d S . .
H2WA H -0.4687 -0.1029 0.4369 0.064 Uiso 0.50 1 d PR . .
H2WB H -0.5000 -0.2198 0.5000 0.064 Uiso 1 2 d SR . .
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
Fe1 0.0233(4) 0.0128(4) 0.0138(4) 0.000 0.0102(3) 0.000
Cu1 0.0299(3) 0.0095(3) 0.0184(3) 0.00083(16) 0.0142(2) -0.00143(17)
C1 0.0228(14) 0.0132(13) 0.0133(13) -0.0022(10) 0.0065(10) -0.0009(10)
C2 0.0195(12) 0.0142(12) 0.0124(12) 0.0015(10) 0.0059(9) -0.0009(10)
N1 0.0219(11) 0.0099(11) 0.0176(12) 0.0003(8) 0.0092(9) -0.0011(8)
N2 0.0222(15) 0.0109(15) 0.0176(16) 0.000 0.0108(13) 0.000
O1W 0.0300(16) 0.0304(16) 0.0188(15) 0.000 0.0095(12) 0.000
O1 0.0373(12) 0.0128(10) 0.0219(11) 0.0018(7) 0.0170(9) 0.0008(7)
O2 0.0362(11) 0.0169(10) 0.0195(10) 0.0012(8) 0.0165(8) 0.0020(8)
O2W 0.059(2) 0.0203(17) 0.091(3) 0.000 0.039(2) 0.000
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'
Fe Fe 0.3463 0.8444 '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
_geom_angle_publ_flag
O1W Fe1 O1W 180.0 . 5_556 ?
O1W Fe1 O2 90.01(8) . 6 ?
O1W Fe1 O2 89.99(8) 5_556 6 ?
O1W Fe1 O2 89.99(8) . 2_556 ?
O1W Fe1 O2 90.01(8) 5_556 2_556 ?
O2 Fe1 O2 180.0 6 2_556 ?
O1W Fe1 O2 89.99(8) . 5_556 ?
O1W Fe1 O2 90.01(8) 5_556 5_556 ?
O2 Fe1 O2 83.31(10) 6 5_556 ?
O2 Fe1 O2 96.69(10) 2_556 5_556 ?
O1W Fe1 O2 90.01(8) . . ?
O1W Fe1 O2 89.99(8) 5_556 . ?
O2 Fe1 O2 96.69(10) 6 . ?
O2 Fe1 O2 83.31(10) 2_556 . ?
O2 Fe1 O2 180.0 5_556 . ?
N1 Cu1 N1 180.000(16) . 7 ?
N1 Cu1 O1 97.52(8) . 7 ?
N1 Cu1 O1 82.48(8) 7 7 ?
N1 Cu1 O1 82.48(8) . . ?
N1 Cu1 O1 97.52(8) 7 . ?
O1 Cu1 O1 180.00(10) 7 . ?
O2 C1 O1 123.7(2) . . ?
O2 C1 C2 122.0(2) . . ?
O1 C1 C2 114.2(2) . . ?
N1 C2 C2 105.92(15) . 6 ?
N1 C2 C1 115.7(2) . . ?
C2 C2 C1 137.89(14) 6 . ?
N2 N1 C2 110.5(2) . . ?
N2 N1 Cu1 137.42(18) . . ?
C2 N1 Cu1 111.98(18) . . ?
N1 N2 N1 107.2(3) 6 . ?
Fe1 O1W H1WB 107.5 . . ?
Fe1 O1W H1WA 113.5 . . ?
H1WB O1W H1WA 107.5 . . ?
C1 O1 Cu1 115.17(16) . . ?
C1 O2 Fe1 140.82(18) . . ?
H2WA O2W H2WB 130.8 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O1W 2.103(3) . ?
Fe1 O1W 2.103(3) 5_556 ?
Fe1 O2 2.1116(18) 6 ?
Fe1 O2 2.1116(18) 2_556 ?
Fe1 O2 2.1116(18) 5_556 ?
Fe1 O2 2.1116(18) . ?
Cu1 N1 1.957(2) . ?
Cu1 N1 1.957(2) 7 ?
Cu1 O1 1.975(2) 7 ?
Cu1 O1 1.975(2) . ?
C1 O2 1.239(3) . ?
C1 O1 1.277(3) . ?
C1 C2 1.481(4) . ?
C2 N1 1.354(3) . ?
C2 C2 1.381(5) 6 ?
N1 N2 1.320(3) . ?
N2 N1 1.320(3) 6 ?
O1W H1WB 0.8500 . ?
O1W H1WA 0.8500 . ?
O2W H2WA 0.8500 . ?
O2W H2WB 0.8500 . ?
