#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/93/4339346.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_4339346
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 H14 Cl Cu2 N3 O11'
_chemical_formula_weight         610.85
_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                101.685(14)
_cell_angle_beta                 100.890(14)
_cell_angle_gamma                98.156(14)
_cell_formula_units_Z            2
_cell_length_a                   8.5757(14)
_cell_length_b                   10.2814(17)
_cell_length_c                   12.933(2)
_cell_measurement_temperature    150(2)
_cell_volume                     1077.2(3)
_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 0.957
_diffrn_measured_fraction_theta_max 0.957
_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  0.0341
_diffrn_reflns_av_sigmaI/netI    0.1058
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7666
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.46
_exptl_absorpt_coefficient_mu    2.167
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.719
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSPACK, Oxford Diffraction Ltd'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.883
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             612
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.081
_refine_diff_density_min         -1.113
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.793
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         6024
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.794
_refine_ls_R_factor_all          0.0849
_refine_ls_R_factor_gt           0.0462
_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)+(0.0861P)²+0.0000P] where P=(Fo²+2Fc²)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1211
_refine_ls_wR_factor_ref         0.1298
_reflns_number_gt                3532
_reflns_number_total             6024
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701440x-file001.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C18 H14 Cl Cu2 N3 O11 '
_cod_database_code               4339346
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
C22 C 0.6775(4) 0.0763(4) 0.5352(3) 0.0175(8) Uani 1 1 d .
C23 C 0.6811(4) 0.1866(4) 0.6330(3) 0.0166(8) Uani 1 1 d .
C24 C 0.7720(5) 0.1959(4) 0.7343(3) 0.0214(9) Uani 1 1 d .
H24 H 0.8365 0.1325 0.7463 0.026 Uiso 1 1 calc R
C25 C 0.7665(5) 0.3013(5) 0.8187(4) 0.0269(10) Uani 1 1 d .
H25 H 0.8274 0.3098 0.8881 0.032 Uiso 1 1 calc R
C26 C 0.6693(5) 0.3934(5) 0.7983(4) 0.0290(10) Uani 1 1 d .
H26 H 0.6642 0.4648 0.8538 0.035 Uiso 1 1 calc R
C27 C 0.5793(5) 0.3787(4) 0.6939(4) 0.0237(9) Uani 1 1 d .
H27 H 0.5134 0.4405 0.6803 0.028 Uiso 1 1 calc R
C32 C 0.2141(5) 0.3495(4) 0.3915(3) 0.0162(8) Uani 1 1 d .
C33 C 0.2286(5) 0.2550(4) 0.2899(3) 0.0171(8) Uani 1 1 d .
C34 C 0.1236(5) 0.2363(4) 0.1908(3) 0.0208(9) Uani 1 1 d .
H34 H 0.0397 0.2843 0.1829 0.025 Uiso 1 1 calc R
C35 C 0.1469(5) 0.1433(5) 0.1026(4) 0.0261(10) Uani 1 1 d .
H35 H 0.0780 0.1275 0.0347 0.031 Uiso 1 1 calc R
C36 C 0.2736(5) 0.0754(5) 0.1179(4) 0.0260(10) Uani 1 1 d .
H36 H 0.2910 0.0131 0.0601 0.031 Uiso 1 1 calc R
C37 C 0.3750(5) 0.1002(4) 0.2195(3) 0.0201(9) Uani 1 1 d .
H37 H 0.4601 0.0537 0.2292 0.024 Uiso 1 1 calc R
C43 C 0.1386(4) 0.2147(4) 0.6787(3) 0.0148(8) Uani 1 1 d .
C47 C 0.1824(5) 0.0143(4) 0.7251(3) 0.0193(8) Uani 1 1 d .
H47 H 0.1685 -0.0795 0.7064 0.023 Uiso 1 1 calc R
C46 C 0.2686(5) 0.0838(4) 0.8277(4) 0.0233(9) Uani 1 1 d .
H46 H 0.3134 0.0375 0.8771 0.028 Uiso 1 1 calc R
C45 C 0.2872(5) 0.2237(5) 0.8560(4) 0.0259(10) Uani 1 1 d .
H45 H 0.3432 0.2722 0.9249 0.031 Uiso 1 1 calc R
C44 C 0.2208(5) 0.2905(4) 0.7795(3) 0.0208(9) Uani 1 1 d .
H44 H 0.2318 0.3842 0.7964 0.025 Uiso 1 1 calc R
C42 C 0.0630(4) 0.2732(4) 0.5874(3) 0.0145(8) Uani 1 1 d .
O33 O 0.0942(3) 0.4059(3) 0.3865(2) 0.0179(6) Uani 1 1 d .
O21 O 0.5984(3) 0.0879(3) 0.4440(2) 0.0169(6) Uani 1 1 d .
O23 O 0.7490(3) -0.0186(3) 0.5485(2) 0.0199(6) Uani 1 1 d .
O31 O 0.3282(3) 0.3639(3) 0.4750(2) 0.0178(6) Uani 1 1 d .
N48 N 0.1184(4) 0.0785(3) 0.6518(3) 0.0141(7) Uani 1 1 d .
O41 O -0.0071(3) 0.1918(3) 0.4987(2) 0.0158(6) Uani 1 1 d .
O43 O 0.0748(3) 0.3994(3) 0.6066(2) 0.0170(6) Uani 1 1 d .
O100 O 0.6962(4) 0.3744(3) 0.4187(2) 0.0234(6) Uani 1 1 d D
H1 H 0.695(6) 0.351(4) 0.3516(18) 0.028 Uiso 1 1 d D
H2 H 0.684(6) 0.456(2) 0.437(3) 0.028 Uiso 1 1 d D
Cu1 Cu 0.0000 0.0000 0.5000 0.01353(15) Uani 1 2 d S
Cu2 Cu 0.47855(6) 0.23592(5) 0.45666(4) 0.01623(13) Uani 1 1 d .
Cu3 Cu 0.0000 0.5000 0.5000 0.01467(16) Uani 1 2 d S
N28 N 0.5856(4) 0.2767(3) 0.6124(3) 0.0187(7) Uani 1 1 d .
N38 N 0.3534(4) 0.1893(3) 0.3039(3) 0.0154(7) Uani 1 1 d .
O11 O 0.7282(4) 0.2559(3) 0.2094(3) 0.0307(7) Uani 1 1 d .
O12 O 0.6001(4) 0.1802(3) 0.0251(3) 0.0358(8) Uani 1 1 d .
O13 O 0.7956(4) 0.3802(4) 0.0854(3) 0.0395(9) Uani 1 1 d .
O14 O 0.5429(4) 0.3751(4) 0.1306(3) 0.0403(9) Uani 1 1 d .
Cl1 Cl 0.66670(12) 0.29810(10) 0.11190(8) 0.0217(2) 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'
S S 0.1246 0.1234 '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'
Cl Cl 0.1484 0.1585 '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'
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
O23 C22 O21 125.0(4) . .
O23 C22 C23 118.6(4) . .
O21 C22 C23 116.3(3) . .
N28 C23 C24 122.3(4) . .
N28 C23 C22 114.2(4) . .
C24 C23 C22 123.5(4) . .
C23 C24 C25 118.9(4) . .
C23 C24 H24 120.5 . .
C25 C24 H24 120.5 . .
C26 C25 C24 119.1(4) . .
C26 C25 H25 120.5 . .
C24 C25 H25 120.5 . .
C25 C26 C27 119.4(4) . .
C25 C26 H26 120.3 . .
C27 C26 H26 120.3 . .
N28 C27 C26 121.3(4) . .
N28 C27 H27 119.4 . .
C26 C27 H27 119.4 . .
O33 C32 O31 126.5(4) . .
O33 C32 C33 117.6(4) . .
O31 C32 C33 115.8(3) . .
C34 C33 N38 122.6(4) . .
C34 C33 C32 123.3(4) . .
N38 C33 C32 114.1(3) . .
C33 C34 C35 118.2(4) . .
C33 C34 H34 120.9 . .
C35 C34 H34 120.9 . .
C34 C35 C36 118.9(4) . .
C34 C35 H35 120.6 . .
C36 C35 H35 120.6 . .
C37 C36 C35 119.8(4) . .
C37 C36 H36 120.1 . .
C35 C36 H36 120.1 . .
N38 C37 C36 121.5(4) . .
N38 C37 H37 119.2 . .
C36 C37 H37 119.2 . .
N48 C43 C44 122.4(4) . .
N48 C43 C42 113.3(3) . .
C44 C43 C42 124.3(4) . .
N48 C47 C46 121.7(4) . .
N48 C47 H47 119.1 . .
C46 C47 H47 119.1 . .
C47 C46 C45 119.0(4) . .
C47 C46 H46 120.5 . .
C45 C46 H46 120.5 . .
C44 C45 C46 119.1(4) . .
C44 C45 H45 120.4 . .
C46 C45 H45 120.4 . .
C45 C44 C43 118.4(4) . .
C45 C44 H44 120.8 . .
C43 C44 H44 120.8 . .
O43 C42 O41 125.3(4) . .
O43 C42 C43 117.1(4) . .
O41 C42 C43 117.6(3) . .
C32 O33 Cu3 131.5(3) . .
C22 O21 Cu2 113.6(3) . .
C22 O23 Cu1 113.8(2) . 1_655
C32 O31 Cu2 114.2(2) . .
C43 N48 C47 119.2(4) . .
C43 N48 Cu1 112.6(3) . .
C47 N48 Cu1 128.2(3) . .
C42 O41 Cu1 113.4(2) . .
C42 O43 Cu3 124.9(3) . .
Cu2 O100 H1 109(3) . .
Cu2 O100 H2 107(3) . .
H1 O100 H2 112(3) . .
O41 Cu1 O41 180.0 . 2_556
O41 Cu1 N48 83.21(12) . .
O41 Cu1 N48 96.79(12) 2_556 .
O41 Cu1 N48 96.79(12) . 2_556
O41 Cu1 N48 83.21(12) 2_556 2_556
N48 Cu1 N48 180.0 . 2_556
O41 Cu1 O23 88.84(10) . 1_455
O41 Cu1 O23 91.16(10) 2_556 1_455
N48 Cu1 O23 92.28(11) . 1_455
N48 Cu1 O23 87.72(11) 2_556 1_455
O41 Cu1 O23 91.16(10) . 2_656
O41 Cu1 O23 88.84(10) 2_556 2_656
N48 Cu1 O23 87.72(11) . 2_656
N48 Cu1 O23 92.28(11) 2_556 2_656
O23 Cu1 O23 180.0 1_455 2_656
O21 Cu2 O31 170.17(11) . .
O21 Cu2 N28 84.29(13) . .
O31 Cu2 N28 95.21(13) . .
O21 Cu2 N38 97.21(13) . .
O31 Cu2 N38 82.49(12) . .
N28 Cu2 N38 175.03(13) . .
O21 Cu2 O100 89.05(11) . .
O31 Cu2 O100 100.78(11) . .
N28 Cu2 O100 91.68(12) . .
N38 Cu2 O100 93.07(12) . .
O43 Cu3 O43 180.000(1) . 2_566
O43 Cu3 O33 95.51(11) . .
O43 Cu3 O33 84.49(11) 2_566 .
O43 Cu3 O33 84.49(11) . 2_566
O43 Cu3 O33 95.51(11) 2_566 2_566
O33 Cu3 O33 180.000(1) . 2_566
C23 N28 C27 119.0(4) . .
C23 N28 Cu2 111.2(3) . .
C27 N28 Cu2 129.8(3) . .
C37 N38 C33 119.1(3) . .
C37 N38 Cu2 128.3(3) . .
C33 N38 Cu2 112.6(3) . .
O13 Cl1 O11 109.3(2) . .
O13 Cl1 O14 109.6(2) . .
O11 Cl1 O14 108.9(2) . .
O13 Cl1 O12 110.1(2) . .
O11 Cl1 O12 109.0(2) . .
O14 Cl1 O12 109.9(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C22 O23 1.247(4) .
C22 O21 1.282(5) .
C22 C23 1.510(6) .
C23 N28 1.354(5) .
C23 C24 1.369(6) .
C24 C25 1.387(6) .
C24 H24 0.9300 .
C25 C26 1.379(6) .
C25 H25 0.9300 .
C26 C27 1.389(6) .
C26 H26 0.9300 .
C27 N28 1.343(5) .
C27 H27 0.9300 .
C32 O33 1.248(4) .
C32 O31 1.280(5) .
C32 C33 1.505(6) .
C33 C34 1.380(6) .
C33 N38 1.347(5) .
C34 C35 1.399(6) .
C34 H34 0.9300 .
C35 C36 1.377(6) .
C35 H35 0.9300 .
C36 C37 1.385(6) .
C36 H36 0.9300 .
C37 N38 1.337(5) .
C37 H37 0.9300 .
C43 N48 1.350(5) .
C43 C44 1.374(6) .
C43 C42 1.512(5) .
C47 N48 1.340(5) .
C47 C46 1.384(6) .
C47 H47 0.9300 .
C46 C45 1.389(6) .
C46 H46 0.9300 .
C45 C44 1.395(6) .
C45 H45 0.9300 .
C44 H44 0.9300 .
C42 O43 1.256(4) .
C42 O41 1.260(5) .
O33 Cu3 1.958(3) .
O21 Cu2 1.950(3) .
O23 Cu1 2.346(3) 1_655
O31 Cu2 1.980(3) .
N48 Cu1 1.977(3) .
O41 Cu1 1.985(3) .
O43 Cu3 1.953(3) .
O100 Cu2 2.371(3) .
O100 H1 0.852(18) .
O100 H2 0.855(18) .
Cu1 O41 1.985(3) 2_556
Cu1 N48 1.977(3) 2_556
Cu1 O23 2.346(3) 1_455
Cu1 O23 2.346(3) 2_656
Cu2 N28 1.981(4) .
Cu2 N38 1.988(3) .
Cu3 O43 1.953(3) 2_566
Cu3 O33 1.958(3) 2_566
O11 Cl1 1.446(3) .
O12 Cl1 1.438(3) .
O13 Cl1 1.431(3) .
O14 Cl1 1.439(3) .
