#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/93/4339345.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_4339345
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 B Cu2 F4 N3 O7'
_chemical_formula_weight         598.21
_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                102.132(12)
_cell_angle_beta                 101.182(11)
_cell_angle_gamma                97.946(10)
_cell_formula_units_Z            2
_cell_length_a                   8.5487(10)
_cell_length_b                   10.2220(13)
_cell_length_c                   12.8509(19)
_cell_measurement_temperature    150(2)
_cell_volume                     1058.1(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 0.951
_diffrn_measured_fraction_theta_max 0.951
_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  0.0560
_diffrn_reflns_av_sigmaI/netI    0.2036
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7436
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.64
_exptl_absorpt_coefficient_mu    2.093
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.749
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSPACK, Oxford Diffraction Ltd'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.878
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             596
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.289
_refine_diff_density_min         -0.982
_refine_diff_density_rms         0.192
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.900
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         5854
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.900
_refine_ls_R_factor_all          0.1186
_refine_ls_R_factor_gt           0.0585
_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          0.1363
_refine_ls_wR_factor_ref         0.1679
_reflns_number_gt                2941
_reflns_number_total             5854
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701440x-file002.cif
_cod_data_source_block           2
_cod_original_cell_volume        1058.1(2)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C18 H14 B Cu2 F4 N3 O7 '
_cod_database_code               4339345
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 0.6768(7) 0.0778(5) 0.5374(5) 0.0209(12) Uani 1 1 d .
C23 C 0.6816(7) 0.1882(5) 0.6346(4) 0.0194(12) Uani 1 1 d .
C24 C 0.7731(7) 0.1989(6) 0.7383(5) 0.0268(13) Uani 1 1 d .
H24 H 0.8380 0.1354 0.7510 0.032 Uiso 1 1 calc R
C25 C 0.7666(7) 0.3057(6) 0.8230(5) 0.0283(14) Uani 1 1 d .
H25 H 0.8263 0.3147 0.8936 0.034 Uiso 1 1 calc R
C26 C 0.6694(8) 0.3986(6) 0.8005(5) 0.0351(16) Uani 1 1 d .
H26 H 0.6656 0.4725 0.8557 0.042 Uiso 1 1 calc R
C27 C 0.5783(8) 0.3811(6) 0.6955(5) 0.0279(14) Uani 1 1 d .
H27 H 0.5095 0.4415 0.6815 0.034 Uiso 1 1 calc R
C32 C 0.2130(6) 0.3486(5) 0.3904(4) 0.0164(11) Uani 1 1 d .
C33 C 0.2267(7) 0.2531(5) 0.2869(4) 0.0200(12) Uani 1 1 d .
C34 C 0.1221(8) 0.2333(5) 0.1895(4) 0.0233(13) Uani 1 1 d .
H34 H 0.0351 0.2787 0.1825 0.028 Uiso 1 1 calc R
C35 C 0.1473(8) 0.1439(6) 0.1003(5) 0.0316(15) Uani 1 1 d .
H35 H 0.0811 0.1312 0.0311 0.038 Uiso 1 1 calc R
C36 C 0.2754(8) 0.0728(6) 0.1168(5) 0.0266(13) Uani 1 1 d .
H36 H 0.2908 0.0076 0.0592 0.032 Uiso 1 1 calc R
C37 C 0.3771(7) 0.0998(5) 0.2177(5) 0.0250(13) Uani 1 1 d .
H37 H 0.4643 0.0548 0.2273 0.030 Uiso 1 1 calc R
C43 C 0.1421(7) 0.2152(5) 0.6806(4) 0.0163(11) Uani 1 1 d .
C47 C 0.1857(7) 0.0132(5) 0.7269(5) 0.0221(12) Uani 1 1 d .
H47 H 0.1714 -0.0813 0.7084 0.027 Uiso 1 1 calc R
C46 C 0.2732(7) 0.0845(5) 0.8293(5) 0.0248(13) Uani 1 1 d .
H46 H 0.3192 0.0386 0.8791 0.030 Uiso 1 1 calc R
C45 C 0.2931(7) 0.2267(6) 0.8584(5) 0.0270(13) Uani 1 1 d .
H45 H 0.3498 0.2761 0.9280 0.032 Uiso 1 1 calc R
C44 C 0.2272(8) 0.2915(6) 0.7822(5) 0.0272(14) Uani 1 1 d .
H44 H 0.2399 0.3859 0.7991 0.033 Uiso 1 1 calc R
C42 C 0.0659(7) 0.2738(5) 0.5898(5) 0.0207(12) Uani 1 1 d .
O33 O 0.0915(5) 0.4038(4) 0.3857(3) 0.0210(8) Uani 1 1 d .
O21 O 0.5988(5) 0.0872(4) 0.4449(3) 0.0229(9) Uani 1 1 d .
O23 O 0.7499(5) -0.0182(4) 0.5517(3) 0.0223(9) Uani 1 1 d .
O31 O 0.3283(5) 0.3641(3) 0.4748(3) 0.0199(8) Uani 1 1 d .
N48 N 0.1199(5) 0.0781(4) 0.6524(4) 0.0183(10) Uani 1 1 d .
O41 O -0.0081(5) 0.1898(3) 0.4997(3) 0.0198(8) Uani 1 1 d .
O43 O 0.0771(5) 0.4017(3) 0.6072(3) 0.0211(8) Uani 1 1 d .
O100 O 0.6957(5) 0.3718(3) 0.4180(3) 0.0246(9) Uani 1 1 d D
H1 H 0.703(8) 0.322(4) 0.357(3) 0.030 Uiso 1 1 d D
H2 H 0.690(7) 0.454(2) 0.415(4) 0.030 Uiso 1 1 d D
Cu1 Cu 0.0000 0.0000 0.5000 0.0171(2) Uani 1 2 d S
Cu2 Cu 0.47885(8) 0.23623(6) 0.45667(6) 0.01915(19) Uani 1 1 d .
Cu3 Cu 0.0000 0.5000 0.5000 0.0177(2) Uani 1 2 d S
N28 N 0.5871(6) 0.2780(4) 0.6129(4) 0.0229(11) Uani 1 1 d .
N38 N 0.3547(5) 0.1891(4) 0.3029(4) 0.0178(10) Uani 1 1 d .
F11 F 0.7236(5) 0.2577(4) 0.2096(3) 0.0381(9) Uani 1 1 d .
F12 F 0.6003(5) 0.1773(3) 0.0311(3) 0.0399(10) Uani 1 1 d .
F13 F 0.7930(5) 0.3706(4) 0.0867(3) 0.0501(11) Uani 1 1 d .
F14 F 0.5485(5) 0.3726(4) 0.1280(3) 0.0497(11) Uani 1 1 d .
B1 B 0.6694(9) 0.2955(7) 0.1135(7) 0.0336(18) 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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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 124.5(5) . .
O23 C22 C23 118.1(5) . .
O21 C22 C23 117.4(5) . .
N28 C23 C24 122.3(5) . .
N28 C23 C22 113.6(5) . .
C24 C23 C22 124.1(5) . .
C23 C24 C25 119.0(6) . .
C23 C24 H24 120.5 . .
C25 C24 H24 120.5 . .
C26 C25 C24 118.7(6) . .
C26 C25 H25 120.6 . .
C24 C25 H25 120.6 . .
C27 C26 C25 119.6(6) . .
C27 C26 H26 120.2 . .
C25 C26 H26 120.2 . .
N28 C27 C26 121.3(6) . .
N28 C27 H27 119.3 . .
C26 C27 H27 119.3 . .
O33 C32 O31 126.5(5) . .
O33 C32 C33 117.3(5) . .
O31 C32 C33 116.2(5) . .
C34 C33 N38 123.8(5) . .
C34 C33 C32 123.5(5) . .
N38 C33 C32 112.7(5) . .
C33 C34 C35 118.4(6) . .
C33 C34 H34 120.8 . .
C35 C34 H34 120.8 . .
C34 C35 C36 118.3(6) . .
C34 C35 H35 120.8 . .
C36 C35 H35 120.8 . .
C37 C36 C35 119.7(5) . .
C37 C36 H36 120.2 . .
C35 C36 H36 120.2 . .
N38 C37 C36 121.7(6) . .
N38 C37 H37 119.2 . .
C36 C37 H37 119.2 . .
N48 C43 C44 122.6(5) . .
N48 C43 C42 113.0(4) . .
C44 C43 C42 124.4(5) . .
N48 C47 C46 121.2(5) . .
N48 C47 H47 119.4 . .
C46 C47 H47 119.4 . .
C47 C46 C45 119.7(5) . .
C47 C46 H46 120.1 . .
C45 C46 H46 120.1 . .
C44 C45 C46 118.7(5) . .
C44 C45 H45 120.7 . .
C46 C45 H45 120.7 . .
C45 C44 C43 119.2(5) . .
C45 C44 H44 120.4 . .
C43 C44 H44 120.4 . .
O43 C42 O41 124.3(5) . .
O43 C42 C43 118.7(5) . .
O41 C42 C43 117.0(5) . .
C32 O33 Cu3 131.5(4) . .
C22 O21 Cu2 112.9(4) . .
C22 O23 Cu1 113.1(3) . 1_655
C32 O31 Cu2 114.3(3) . .
C43 N48 C47 118.6(5) . .
C43 N48 Cu1 112.7(3) . .
C47 N48 Cu1 128.6(4) . .
C42 O41 Cu1 113.7(3) . .
C42 O43 Cu3 125.8(4) . .
Cu2 O100 H1 101(4) . .
Cu2 O100 H2 120(4) . .
H1 O100 H2 112(3) . .
O41 Cu1 O41 180.0 . 2_556
O41 Cu1 N48 83.52(16) . .
O41 Cu1 N48 96.48(16) 2_556 .
O41 Cu1 N48 96.48(16) . 2_556
O41 Cu1 N48 83.52(16) 2_556 2_556
N48 Cu1 N48 180.0 . 2_556
O41 Cu1 O23 88.84(14) . 1_455
O41 Cu1 O23 91.16(14) 2_556 1_455
N48 Cu1 O23 91.62(16) . 1_455
N48 Cu1 O23 88.38(16) 2_556 1_455
O41 Cu1 O23 91.16(14) . 2_656
O41 Cu1 O23 88.84(14) 2_556 2_656
N48 Cu1 O23 88.38(16) . 2_656
N48 Cu1 O23 91.62(16) 2_556 2_656
O23 Cu1 O23 180.0 1_455 2_656
O21 Cu2 O31 169.78(15) . .
O21 Cu2 N28 83.83(18) . .
O31 Cu2 N28 95.45(18) . .
O21 Cu2 N38 97.41(17) . .
O31 Cu2 N38 82.58(17) . .
N28 Cu2 N38 175.61(19) . .
O21 Cu2 O100 88.77(15) . .
O31 Cu2 O100 101.45(15) . .
N28 Cu2 O100 91.85(16) . .
N38 Cu2 O100 92.39(16) . .
O43 Cu3 O43 180.000(1) . 2_566
O43 Cu3 O33 95.63(15) . .
O43 Cu3 O33 84.37(15) 2_566 .
O43 Cu3 O33 84.37(15) . 2_566
O43 Cu3 O33 95.63(15) 2_566 2_566
O33 Cu3 O33 180.000(2) . 2_566
C23 N28 C27 119.0(5) . .
C23 N28 Cu2 111.8(4) . .
C27 N28 Cu2 129.2(4) . .
C37 N38 C33 118.0(5) . .
C37 N38 Cu2 128.4(4) . .
C33 N38 Cu2 113.5(3) . .
F13 B1 F11 110.9(6) . .
F13 B1 F12 111.2(6) . .
F11 B1 F12 108.2(6) . .
F13 B1 F14 109.6(6) . .
F11 B1 F14 108.5(6) . .
F12 B1 F14 108.3(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C22 O23 1.261(6) .
C22 O21 1.274(7) .
C22 C23 1.487(8) .
C23 N28 1.341(7) .
C23 C24 1.382(8) .
C24 C25 1.386(8) .
C24 H24 0.9300 .
C25 C26 1.385(9) .
C25 H25 0.9300 .
C26 C27 1.383(9) .
C26 H26 0.9300 .
C27 N28 1.352(7) .
C27 H27 0.9300 .
C32 O33 1.246(6) .
C32 O31 1.282(6) .
C32 C33 1.511(7) .
C33 C34 1.348(8) .
C33 N38 1.354(7) .
C34 C35 1.379(8) .
C34 H34 0.9300 .
C35 C36 1.402(9) .
C35 H35 0.9300 .
C36 C37 1.364(8) .
C36 H36 0.9300 .
C37 N38 1.334(6) .
C37 H37 0.9300 .
C43 N48 1.347(6) .
C43 C44 1.375(8) .
C43 C42 1.500(8) .
C47 N48 1.355(7) .
C47 C46 1.373(8) .
C47 H47 0.9300 .
C46 C45 1.399(8) .
C46 H46 0.9300 .
C45 C44 1.369(8) .
C45 H45 0.9300 .
C44 H44 0.9300 .
C42 O43 1.266(6) .
C42 O41 1.275(6) .
O33 Cu3 1.946(4) .
O21 Cu2 1.947(4) .
O23 Cu1 2.354(4) 1_655
O31 Cu2 1.968(4) .
N48 Cu1 1.965(4) .
O41 Cu1 1.951(3) .
O43 Cu3 1.938(4) .
O100 Cu2 2.354(4) .
O100 H1 0.860(19) .
O100 H2 0.858(19) .
Cu1 O41 1.951(3) 2_556
Cu1 N48 1.965(4) 2_556
Cu1 O23 2.354(4) 1_455
Cu1 O23 2.354(4) 2_656
Cu2 N28 1.970(5) .
Cu2 N38 1.977(4) .
Cu3 O43 1.938(4) 2_566
Cu3 O33 1.946(4) 2_566
F11 B1 1.385(9) .
F12 B1 1.397(8) .
F13 B1 1.360(9) .
F14 B1 1.401(8) .
