#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:22:32 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180036 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/30/7033086.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_7033086
loop_
_publ_author_name
'Davenport, T. C.'
'Tilley, T. D.'
_publ_section_title
;
 Dinuclear first-row transition metal complexes with a naphthyridine-based
 dinucleating ligand.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12244
_journal_page_last               12255
_journal_paper_doi               10.1039/c4dt02727b
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety
'C60 H40 Cl6 Cu4 F4 N12 2+, 2(Cl 1-), 2(C H4 O), 2(C4 H8 O)'
_chemical_formula_sum            'C70 H64 Cl8 Cu4 F4 N12 O4'
_chemical_formula_weight         1751.15
_chemical_name_common            '[Cu4(u-Cl)6(DPFN)2][Cl]2'
_chemical_name_systematic
;
 ?
;
_chemical_properties_physical    Hygroscopic
_space_group_IT_number           70
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-F 2uv 2vw'
_symmetry_space_group_name_H-M   'F d d d :2'
_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                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.1594(6)
_cell_length_b                   21.5153(8)
_cell_length_c                   43.7045(17)
_cell_measurement_reflns_used    9886
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.38
_cell_measurement_theta_min      2.84
_cell_volume                     14254.6(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-I CCD'
_diffrn_measurement_method       'φ and ω 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  0.0429
_diffrn_reflns_av_sigmaI/netI    0.0228
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            44697
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.34
_diffrn_reflns_theta_min         1.71
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.547
_exptl_absorpt_correction_T_max  0.8620
_exptl_absorpt_correction_T_min  0.7783
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             7104
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: ethanol, diethylether'
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.183
_refine_diff_density_min         -0.567
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         3262
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0488
_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)+(0.0609P)²+229.9214P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1318
_refine_ls_wR_factor_ref         0.1526
_reflns_number_gt                2262
_reflns_number_total             3262
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c4dt02727b1.cif
_cod_data_source_block           '[Cu4(u-Cl)6(DPFN)2][Cl]2'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2827 2014-09-09 07:05:25Z andrius 

 Adding full bibliography for 7033083--7033087.cif.
;
_cod_original_sg_symbol_H-M      Fddd
_cod_database_code               7033086
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+3/4, -y+3/4, z'
'-x+3/4, y, -z+3/4'
'x, -y+3/4, -z+3/4'
'x, y+1/2, z+1/2'
'-x+3/4, -y+5/4, z+1/2'
'-x+3/4, y+1/2, -z+5/4'
'x, -y+5/4, -z+5/4'
'x+1/2, y, z+1/2'
'-x+5/4, -y+3/4, z+1/2'
'-x+5/4, y, -z+5/4'
'x+1/2, -y+3/4, -z+5/4'
'x+1/2, y+1/2, z'
'-x+5/4, -y+5/4, z'
'-x+5/4, y+1/2, -z+3/4'
'x+1/2, -y+5/4, -z+3/4'
'-x, -y, -z'
'x-3/4, y-3/4, -z'
'x-3/4, -y, z-3/4'
'-x, y-3/4, z-3/4'
'-x, -y+1/2, -z+1/2'
'x-3/4, y-1/4, -z+1/2'
'x-3/4, -y+1/2, z-1/4'
'-x, y-1/4, z-1/4'
'-x+1/2, -y, -z+1/2'
'x-1/4, y-3/4, -z+1/2'
'x-1/4, -y, z-1/4'
'-x+1/2, y-3/4, z-1/4'
'-x+1/2, -y+1/2, -z'
'x-1/4, y-1/4, -z'
'x-1/4, -y+1/2, z-3/4'
'-x+1/2, y-1/4, z-3/4'
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
C1 C 0.6291(5) 0.8845(2) 0.07245(12) 0.0573(18) Uani 1 1 d . . .
C2 C 0.6306(7) 0.9498(3) 0.07036(14) 0.102(4) Uani 1 1 d . . .
H2 H 0.6326 0.9700 0.0510 0.122 Uiso 1 1 calc R . .
C3 C 0.6292(9) 0.9829(3) 0.09658(16) 0.136(5) Uani 1 1 d . . .
H3 H 0.6310 1.0270 0.0960 0.163 Uiso 1 1 calc R . .
C4 C 0.6250 0.9516(4) 0.1250 0.093(5) Uani 1 2 d S . .
C5 C 0.6250 0.8860(3) 0.1250 0.054(2) Uani 1 2 d S . .
C6 C 0.6307(5) 0.8461(2) 0.04261(11) 0.0519(16) Uani 1 1 d . . .
C7 C 0.7147(4) 0.8078(2) 0.03959(11) 0.0436(14) Uani 1 1 d . . .
C8 C 0.7804(5) 0.8220(3) 0.01837(12) 0.059(2) Uani 1 1 d . . .
H8 H 0.7734 0.8562 0.0048 0.071 Uiso 1 1 calc R . .
C9 C 0.8553(5) 0.7863(3) 0.01715(14) 0.060(2) Uani 1 1 d . . .
H9 H 0.9007 0.7959 0.0029 0.072 Uiso 1 1 calc R . .
C10 C 0.8645(4) 0.7369(3) 0.03654(12) 0.0508(16) Uani 1 1 d . . .
H10 H 0.9159 0.7117 0.0360 0.061 Uiso 1 1 calc R . .
C11 C 0.7967(4) 0.7245(3) 0.05700(11) 0.0419(13) Uani 1 1 d . . .
H11 H 0.8027 0.6902 0.0705 0.050 Uiso 1 1 calc R . .
C12 C 0.5461(4) 0.8090(2) 0.03891(11) 0.0424(14) Uani 1 1 d . . .
C13 C 0.4848(5) 0.8247(3) 0.01708(12) 0.0522(16) Uani 1 1 d . . .
H13 H 0.4941 0.8595 0.0041 0.063 Uiso 1 1 calc R . .
C14 C 0.4096(5) 0.7890(3) 0.01435(13) 0.0596(19) Uani 1 1 d . . .
H14 H 0.3666 0.7991 -0.0007 0.072 Uiso 1 1 calc R . .
C15 C 0.3968(4) 0.7388(3) 0.03332(13) 0.0499(16) Uani 1 1 d . . .
H15 H 0.3451 0.7140 0.0317 0.060 Uiso 1 1 calc R . .
C16 C 0.4612(4) 0.7251(3) 0.05482(12) 0.0417(13) Uani 1 1 d . . .
H16 H 0.4532 0.6905 0.0680 0.050 Uiso 1 1 calc R . .
N1 N 0.6271(4) 0.85301(19) 0.09839(9) 0.0439(11) Uani 1 1 d . . .
N2 N 0.7225(3) 0.75911(19) 0.05851(8) 0.0367(10) Uani 1 1 d . . .
N3 N 0.5348(3) 0.75960(19) 0.05754(9) 0.0364(10) Uani 1 1 d . . .
F1 F 0.6322(3) 0.88885(14) 0.01864(7) 0.0689(12) Uani 1 1 d . . .
Cl2 Cl 0.6250 0.6250 0.05973(3) 0.0313(4) Uani 1 2 d S . .
Cl1 Cl 0.72851(9) 0.71416(6) 0.12554(3) 0.0394(3) Uani 1 1 d . . .
Cu1 Cu 0.62677(4) 0.73362(3) 0.087926(12) 0.0327(2) Uani 1 1 d . . .
Cl3 Cl 0.5546(4) 0.11665(17) 0.05236(8) 0.0863(16) Uani 0.50 1 d P . 1
C17 C 0.486(2) 0.1167(14) 0.0568(5) 0.17(2) Uani 0.38 1 d PDU A 2
H17A H 0.5262 0.1516 0.0534 0.258 Uiso 0.38 1 calc PR A 2
H17B H 0.4368 0.1192 0.0423 0.258 Uiso 0.38 1 calc PR A 2
H17C H 0.5176 0.0775 0.0538 0.258 Uiso 0.38 1 calc PR A 2
O1 O 0.4508(17) 0.1194(10) 0.0890(4) 0.169(11) Uani 0.38 1 d PDU A 2
H1A H 0.4111 0.0925 0.0912 0.253 Uiso 0.38 1 calc PR A 2
C18 C 0.532(2) 0.1250 0.1250 0.14(3) Uani 0.25 2 d SPDU B 1
H18A H 0.5535 0.0836 0.1306 0.215 Uiso 0.13 1 calc PR B 1
H18B H 0.5535 0.1556 0.1399 0.215 Uiso 0.13 1 calc PR B 1
H18C H 0.5535 0.1359 0.1045 0.215 Uiso 0.13 1 calc PR B 1
O2 O 0.4382(16) 0.1250 0.1250 0.109(14) Uani 0.25 2 d SPDU B 1
H2A H 0.4197 0.0983 0.1125 0.163 Uiso 0.13 1 calc PR B 1
C19 C 0.4067(17) 0.3290(9) 0.1383(4) 0.270(16) Uani 1 1 d . . .
H19A H 0.3796 0.2893 0.1448 0.324 Uiso 1 1 calc R C 1
H19B H 0.4712 0.3258 0.1414 0.324 Uiso 1 1 calc R C 1
C20 C 0.3750 0.3750 0.1553(4) 0.233(17) Uani 1 2 d SD . .
H20A H 0.3275 0.3587 0.1686 0.279 Uiso 0.50 1 calc PR . .
H20B H 0.4225 0.3913 0.1686 0.279 Uiso 0.50 1 calc PR . .
C21 C 0.3884(16) 0.3395(9) 0.1065(3) 0.310(18) Uani 0.50 1 d PD . 1
H21A H 0.3395 0.3129 0.0992 0.372 Uiso 0.50 1 calc PR . 1
H21B H 0.4413 0.3320 0.0937 0.372 Uiso 0.50 1 calc PR . 1
O3 O 0.3884(16) 0.3395(9) 0.1065(3) 0.310(18) Uani 0.50 1 d PD . 2
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'
F F 0.0171 0.0103 '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'
Cu Cu 0.3201 1.2651 '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
N1 C1 C2 124.6(5) . .
N1 C1 C6 116.9(4) . .
C2 C1 C6 118.6(5) . .
C3 C2 C1 118.1(6) . .
C3 C2 H2 121.0 . .
C1 C2 H2 121.0 . .
C2 C3 C4 119.7(6) . .
C2 C3 H3 120.1 . .
C4 C3 H3 120.1 . .
C5 C4 C3 118.4(4) . .
C5 C4 C3 118.4(4) . 11_554
C3 C4 C3 123.1(8) . 11_554
N1 C5 N1 117.2(6) . 11_554
N1 C5 C4 121.4(3) . .
N1 C5 C4 121.4(3) 11_554 .
F1 C6 C12 106.3(5) . .
F1 C6 C7 106.1(5) . .
C12 C6 C7 114.3(4) . .
F1 C6 C1 106.4(4) . .
C12 C6 C1 111.0(5) . .
C7 C6 C1 112.0(5) . .
N2 C7 C8 121.3(6) . .
N2 C7 C6 116.3(5) . .
C8 C7 C6 122.4(5) . .
C9 C8 C7 119.6(6) . .
C9 C8 H8 120.2 . .
C7 C8 H8 120.2 . .
C10 C9 C8 119.7(6) . .
C10 C9 H9 120.2 . .
C8 C9 H9 120.2 . .
C9 C10 C11 118.3(7) . .
C9 C10 H10 120.9 . .
C11 C10 H10 120.9 . .
N2 C11 C10 122.8(6) . .
N2 C11 H11 118.6 . .
C10 C11 H11 118.6 . .
N3 C12 C13 121.8(6) . .
N3 C12 C6 117.2(5) . .
C13 C12 C6 121.0(5) . .
C12 C13 C14 118.8(6) . .
C12 C13 H13 120.6 . .
C14 C13 H13 120.6 . .
C15 C14 C13 120.1(5) . .
C15 C14 H14 120.0 . .
C13 C14 H14 120.0 . .
C14 C15 C16 118.4(6) . .
C14 C15 H15 120.8 . .
C16 C15 H15 120.8 . .
N3 C16 C15 121.8(6) . .
N3 C16 H16 119.1 . .
C15 C16 H16 119.1 . .
C1 N1 C5 117.8(4) . .
C7 N2 C11 118.3(5) . .
C7 N2 Cu1 122.9(4) . .
C11 N2 Cu1 118.8(3) . .
C16 N3 C12 119.1(5) . .
C16 N3 Cu1 118.8(3) . .
C12 N3 Cu1 122.1(4) . .
Cu1 Cl2 Cu1 124.40(6) . 14
Cu1 Cl1 Cu1 89.87(5) . 11_554
N3 Cu1 N2 90.13(17) . .
N3 Cu1 Cl1 173.53(12) . .
N2 Cu1 Cl1 91.31(13) . .
N3 Cu1 Cl1 91.61(13) . 11_554
N2 Cu1 Cl1 173.73(12) . 11_554
Cl1 Cu1 Cl1 86.31(5) . 11_554
N3 Cu1 Cl2 86.02(12) . .
N2 Cu1 Cl2 87.16(12) . .
Cl1 Cu1 Cl2 100.35(4) . .
Cl1 Cu1 Cl2 98.97(4) 11_554 .
O1 C17 H17A 109.5 . .
O1 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
O1 C17 H17C 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
C17 O1 H1A 109.5 . .
O2 C18 H18A 109.5 . .
O2 C18 H18B 109.5 . .
H18A C18 H18B 109.5 . .
O2 C18 H18C 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
C18 O2 H2A 109.5 . .
C20 C19 C21 111(2) . .
C20 C19 H19A 109.5 . .
C21 C19 H19A 109.5 . .
C20 C19 H19B 109.5 . .
C21 C19 H19B 109.5 . .
H19A C19 H19B 108.1 . .
C19 C20 C19 112(2) 2 .
C19 C20 H20A 109.2 2 .
C19 C20 H20A 109.2 . .
C19 C20 H20B 109.2 2 .
C19 C20 H20B 109.2 . .
H20A C20 H20B 107.9 . .
C19 C21 C21 101.6(12) . 2
C19 C21 H21A 111.4 . .
C21 C21 H21A 111.4 2 .
C19 C21 H21B 111.4 . .
C21 C21 H21B 111.4 2 .
H21A C21 H21B 109.3 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.321(7) .
C1 C2 1.410(8) .
C1 C6 1.544(7) .
C2 C3 1.349(9) .
C2 H2 0.9500 .
C3 C4 1.414(8) .
C3 H3 0.9500 .
C4 C5 1.411(11) .
C5 N1 1.363(5) .
C6 F1 1.394(5) .
C6 C12 1.520(9) .
C6 C7 1.523(9) .
C7 N2 1.339(6) .
C7 C8 1.396(8) .
C8 C9 1.372(10) .
C8 H8 0.9500 .
C9 C10 1.367(10) .
C9 H9 0.9500 .
C10 C11 1.388(7) .
C10 H10 0.9500 .
C11 N2 1.350(7) .
C11 H11 0.9500 .
C12 N3 1.349(7) .
C12 C13 1.373(8) .
C13 C14 1.381(10) .
C13 H13 0.9500 .
C14 C15 1.375(9) .
C14 H14 0.9500 .
C15 C16 1.387(7) .
C15 H15 0.9500 .
C16 N3 1.345(7) .
C16 H16 0.9500 .
N2 Cu1 2.015(4) .
N3 Cu1 2.005(4) .
Cl2 Cu1 2.6421(9) .
Cl1 Cu1 2.2927(14) .
C17 O1 1.503(19) .
C17 H17A 0.9800 .
C17 H17B 0.9800 .
C17 H17C 0.9800 .
O1 H1A 0.8400 .
C18 O2 1.42(2) .
C18 H18A 0.9800 .
C18 H18B 0.9800 .
C18 H18C 0.9800 .
O2 H2A 0.8400 .
C19 C20 1.33(2) .
C19 C21 1.44(2) .
C19 H19A 0.9900 .
C19 H19B 0.9900 .
C20 C19 1.33(2) 2
C20 H20A 0.9900 .
C20 H20B 0.9900 .
C21 C21 1.58(5) 2
C21 H21A 0.9900 .
C21 H21B 0.9900 .
