#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:55:38 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179496 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/93/4339344.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_4339344
loop_
_publ_author_name
'Biswas, Chaitali'
'Mukherjee, Pampa'
'Drew, Michael G. B.'
'Gómez-García, Carlos J'
'Clemente-Juan, Juan M'
'Ghosh, Ashutosh'
_publ_section_title
;
 Anion-directed synthesis of metal-organic frameworks based on
 2-picolinate CuII complexes: a ferromagnetic alternating chain and two
 unprecedented ferromagnetic fish backbone chains.
;
_journal_issue                   25
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10771
_journal_page_last               10780
_journal_paper_doi               10.1021/ic701440x
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C18 H16 Cu2 N4 O11'
_chemical_formula_weight         591.42
_chemical_name_systematic
; 

 ? 

;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 99.095(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.9597(4)
_cell_length_b                   15.7704(9)
_cell_length_c                   19.2329(8)
_cell_measurement_temperature    150(2)
_cell_volume                     2084.41(19)
_computing_cell_refinement       'Crysalis, Oxford Diffraction'
_computing_data_collection       'Crysalis, Oxford Diffraction'
_computing_data_reduction        'Crysalis, Oxford Diffraction'
_computing_molecular_graphics    PLATON(Spek,2004)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device       'Oxford Diffaction X-Calibur System'
_diffrn_measurement_method       '321 frames, counting time 10 s.'
_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  0.0564
_diffrn_reflns_av_sigmaI/netI    0.1212
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13449
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.50
_exptl_absorpt_coefficient_mu    2.113
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.785
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSPACK, Oxford Diffraction Ltd'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.885
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.533
_refine_diff_density_min         -0.687
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         5946
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.1187
_refine_ls_R_factor_gt           0.0626
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;

_refine_ls_weighting_details 

  w=1/[σ²(Fo²)+(0.0322P)²+0.0000P] where P=(Fo²+2Fc²)/3 

;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0908
_refine_ls_wR_factor_ref         0.1034
_reflns_number_gt                3577
_reflns_number_total             5946
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701440x-file004.cif
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4339344
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, 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
C12 C 1.3049(6) 0.3058(3) 0.21627(19) 0.0182(9) Uani 1 1 d .
C13 C 1.1735(6) 0.3749(3) 0.23664(18) 0.0162(9) Uani 1 1 d .
C14 C 1.2183(6) 0.4598(3) 0.23839(19) 0.0193(9) Uani 1 1 d .
H14 H 1.3391 0.4781 0.2295 0.023 Uiso 1 1 calc R
C15 C 1.0814(6) 0.5178(3) 0.2536(2) 0.0242(10) Uani 1 1 d .
H15 H 1.1088 0.5756 0.2549 0.029 Uiso 1 1 calc R
C16 C 0.9017(6) 0.4883(3) 0.2669(2) 0.0224(10) Uani 1 1 d .
H16 H 0.8060 0.5261 0.2760 0.027 Uiso 1 1 calc R
C17 C 0.8683(6) 0.4009(3) 0.26638(18) 0.0174(9) Uani 1 1 d .
H17 H 0.7498 0.3810 0.2762 0.021 Uiso 1 1 calc R
C27 C 0.6748(6) 0.0707(3) -0.0595(2) 0.0180(10) Uani 1 1 d .
H27 H 0.6233 0.0963 -0.1020 0.022 Uiso 1 1 calc R
C26 C 0.6862(6) -0.0165(3) -0.0567(2) 0.0202(10) Uani 1 1 d .
H26 H 0.6416 -0.0491 -0.0963 0.024 Uiso 1 1 calc R
C25 C 0.7659(6) -0.0546(3) 0.00643(19) 0.0205(10) Uani 1 1 d .
H25 H 0.7754 -0.1133 0.0098 0.025 Uiso 1 1 calc R
C24 C 0.8306(6) -0.0041(3) 0.0640(2) 0.0157(9) Uani 1 1 d .
H24 H 0.8854 -0.0282 0.1067 0.019 Uiso 1 1 calc R
C23 C 0.8128(6) 0.0823(3) 0.05719(19) 0.0129(9) Uani 1 1 d .
C22 C 0.8788(5) 0.1444(3) 0.11529(19) 0.0135(9) Uani 1 1 d .
C32 C 0.6141(6) 0.3439(3) -0.11154(19) 0.0151(9) Uani 1 1 d .
C33 C 0.6819(6) 0.4054(2) -0.05318(19) 0.0124(8) Uani 1 1 d .
C34 C 0.6838(6) 0.4925(3) -0.0610(2) 0.0209(10) Uani 1 1 d .
H34 H 0.6407 0.5177 -0.1044 0.025 Uiso 1 1 calc R
C35 C 0.7521(6) 0.5414(3) -0.0020(2) 0.0226(11) Uani 1 1 d .
H35 H 0.7601 0.6001 -0.0059 0.027 Uiso 1 1 calc R
C36 C 0.8078(6) 0.5025(3) 0.0623(2) 0.0217(10) Uani 1 1 d .
H36 H 0.8496 0.5345 0.1024 0.026 Uiso 1 1 calc R
C37 C 0.8004(6) 0.4159(3) 0.0659(2) 0.0216(10) Uani 1 1 d .
H37 H 0.8392 0.3897 0.1091 0.026 Uiso 1 1 calc R
N18 N 1.0017(5) 0.34500(19) 0.25209(16) 0.0138(7) Uani 1 1 d .
N28 N 0.7343(4) 0.1197(2) -0.00417(14) 0.0131(8) Uani 1 1 d .
N38 N 0.7395(5) 0.3677(2) 0.00948(16) 0.0160(8) Uani 1 1 d .
N51 N 0.0722(5) 0.2503(2) 0.90432(16) 0.0201(8) Uani 1 1 d .
O11 O 1.2516(4) 0.23020(18) 0.22496(14) 0.0194(6) Uani 1 1 d .
O13 O 1.4558(4) 0.32686(19) 0.19217(13) 0.0206(7) Uani 1 1 d .
O23 O 0.9527(4) 0.11594(17) 0.17381(12) 0.0147(6) Uani 1 1 d .
O21 O 0.8553(4) 0.22241(18) 0.10064(12) 0.0156(6) Uani 1 1 d .
O33 O 0.5598(4) 0.37238(18) -0.17212(13) 0.0177(6) Uani 1 1 d .
O31 O 0.6161(4) 0.26623(17) -0.09476(12) 0.0182(6) Uani 1 1 d .
O52 O 0.1135(5) 0.3177(2) 0.87624(15) 0.0388(9) Uani 1 1 d .
O53 O 0.0404(5) 0.18522(19) 0.86950(14) 0.0308(8) Uani 1 1 d .
O54 O 0.0645(4) 0.25047(19) 0.97001(13) 0.0218(7) Uani 1 1 d .
O100 O 0.7135(4) 0.20624(19) 0.24991(13) 0.0186(6) Uani 1 1 d D
H1 H 0.692(5) 0.200(2) 0.2926(11) 0.022 Uiso 1 1 d D
H2 H 0.640(5) 0.244(2) 0.2275(16) 0.022 Uiso 1 1 d D
O200 O 0.4354(4) 0.2405(2) 0.05645(14) 0.0276(7) Uani 1 1 d D
H3 H 0.443(5) 0.254(3) 0.1011(10) 0.033 Uiso 1 1 d D
H4 H 0.319(3) 0.247(3) 0.0350(17) 0.033 Uiso 1 1 d D
Cu1 Cu 0.98878(7) 0.21665(3) 0.24435(2) 0.01392(13) Uani 1 1 d .
Cu2 Cu 0.72564(7) 0.24372(3) 0.00363(2) 0.01611(13) 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_3
O13 C12 O11 125.1(4) .
O13 C12 C13 118.7(4) .
O11 C12 C13 116.2(4) .
N18 C13 C14 122.4(4) .
N18 C13 C12 113.3(4) .
C14 C13 C12 124.3(4) .
C13 C14 C15 119.2(4) .
C14 C15 C16 119.0(4) .
C15 C16 C17 118.7(4) .
N18 C17 C16 122.1(4) .
N28 C27 C26 122.7(4) .
C27 C26 C25 118.6(4) .
C24 C25 C26 119.1(4) .
C23 C24 C25 118.8(3) .
N28 C23 C24 122.2(3) .
N28 C23 C22 113.5(3) .
C24 C23 C22 124.3(3) .
O23 C22 O21 124.9(4) .
O23 C22 C23 118.2(4) .
O21 C22 C23 117.0(3) .
O33 C32 O31 125.1(3) .
O33 C32 C33 118.5(4) .
O31 C32 C33 116.4(3) .
N38 C33 C34 122.0(3) .
N38 C33 C32 113.4(3) .
C34 C33 C32 124.6(3) .
C33 C34 C35 118.0(4) .
C36 C35 C34 119.7(4) .
C37 C36 C35 118.8(4) .
N38 C37 C36 122.4(4) .
C17 N18 C13 118.5(4) .
C17 N18 Cu1 130.3(3) .
C13 N18 Cu1 111.1(3) .
C27 N28 C23 118.5(3) .
C27 N28 Cu2 129.2(3) .
C23 N28 Cu2 112.3(2) .
C37 N38 C33 119.1(4) .
C37 N38 Cu2 128.3(3) .
C33 N38 Cu2 112.6(2) .
O53 N51 O52 120.7(3) .
O53 N51 O54 120.8(4) .
O52 N51 O54 118.5(3) .
C12 O11 Cu1 115.7(3) .
C22 O23 Cu1 107.7(3) .
C22 O21 Cu2 113.6(2) .
C32 O33 Cu1 117.7(3) 4_565
C32 O31 Cu2 114.1(2) .
O11 Cu1 O100 171.99(11) .
O11 Cu1 N18 82.64(13) .
O100 Cu1 N18 96.47(13) .
O11 Cu1 O23 88.79(11) .
O100 Cu1 O23 87.30(11) .
N18 Cu1 O23 144.01(11) .
O11 Cu1 O33 95.98(11) 4_666
O100 Cu1 O33 90.93(11) 4_666
N18 Cu1 O33 126.79(11) 4_666
O23 Cu1 O33 88.76(10) 4_666
O31 Cu2 N38 83.26(12) .
O31 Cu2 N28 96.82(11) .
N38 Cu2 N28 175.13(14) .
O31 Cu2 O21 175.69(11) .
N38 Cu2 O21 96.02(12) .
N28 Cu2 O21 83.53(11) .
O31 Cu2 O200 100.82(11) .
N38 Cu2 O200 91.94(13) .
N28 Cu2 O200 92.82(12) .
O21 Cu2 O200 83.44(10) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C12 O13 1.257(5) .
C12 O11 1.268(5) .
C12 C13 1.513(6) .
C13 N18 1.361(5) .
C13 C14 1.375(6) .
C14 C15 1.385(6) .
C15 C16 1.396(6) .
C16 C17 1.397(6) .
C17 N18 1.340(5) .
C27 N28 1.328(5) .
C27 C26 1.377(6) .
C26 C25 1.390(5) .
C25 C24 1.381(5) .
C24 C23 1.373(5) .
C23 N28 1.354(4) .
C23 C22 1.502(5) .
C22 O23 1.245(4) .
C22 O21 1.267(5) .
C32 O33 1.250(4) .
C32 O31 1.266(5) .
C32 C33 1.502(5) .
C33 N38 1.347(4) .
C33 C34 1.382(5) .
C34 C35 1.391(5) .
C35 C36 1.380(5) .
C36 C37 1.368(6) .
C37 N38 1.337(5) .
N18 Cu1 2.031(3) .
N28 Cu2 1.964(3) .
N38 Cu2 1.960(3) .
N51 O53 1.226(4) .
N51 O52 1.246(4) .
N51 O54 1.273(4) .
O11 Cu1 1.936(3) .
O23 Cu1 2.078(3) .
O21 Cu2 1.969(2) .
O33 Cu1 2.132(3) 4_565
O31 Cu2 1.958(2) .
O100 Cu1 1.942(3) .
O200 Cu2 2.401(3) .
Cu1 O33 2.132(3) 4_666
