#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/06/7050625.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_7050625
loop_
_publ_author_name
'van Albada, Gerard A.'
'Roubeau, Olivier'
'Mutikainen, Ilpo'
'Turpeinen, Urho'
'Reedijk, Jan'
_publ_section_title
;
 A unique methoxo- and fluoro-bridged triangular trinuclear Cu(ii)
 species linked in a lattice via mononuclear Cu(ii) units. Synthesis,
 X-ray structure and magnetism of
 [Cu4(2-aminopyrimidine)6(�3-OCH3)2(�-F)3(F)2](BF4)Electronic
 supplementary information (ESI) available: fitting of the magnetic
 coupling according to Scheme 2(a). See
 http://www.rsc.org/suppdata/nj/b3/b304979e/
;
_journal_issue                   12
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1693
_journal_paper_doi               10.1039/b304979e
_journal_volume                  27
_journal_year                    2003
_chemical_formula_moiety         'C26 H36 Cu4 F5 N18 O2, B F4'
_chemical_formula_sum            'C26 H36 B Cu4 F9 N18 O2'
_chemical_formula_weight         1068.70
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 108.64(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.899(6)
_cell_length_b                   21.435(8)
_cell_length_c                   16.727(7)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      7.0
_cell_measurement_theta_min      3.5
_cell_volume                     4043(3)
_computing_cell_refinement       'Rigaku AFC-7S software'
_computing_data_collection       'Rigaku AFC-7S software'
_computing_data_reduction        Texsan
_computing_molecular_graphics    'SHELXTL-PC  V. 5.03 (Sheldrick, 1995)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device_type  'Rigaku AFC-7S'
_diffrn_measurement_method       omega-2theta
_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  0.1482
_diffrn_reflns_av_sigmaI/netI    0.2075
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            7437
_diffrn_reflns_theta_full        25.30
_diffrn_reflns_theta_max         25.30
_diffrn_reflns_theta_min         2.57
_diffrn_standards_decay_%        <2.0
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.170
_exptl_absorpt_correction_T_max  0.897
_exptl_absorpt_correction_T_min  0.683
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
'North etal. (1968). Acta Cryst. A24, 351-359'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.756
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2144
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.866
_refine_diff_density_min         -0.655
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.902
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         3654
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.902
_refine_ls_R_factor_all          0.1752
_refine_ls_R_factor_gt           0.0735
_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)+(0.0528P)²+0.0000P] where P==(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1402
_refine_ls_wR_factor_ref         0.1711
_reflns_number_gt                1623
_reflns_number_total             3654
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b304979e.txt
_cod_data_source_block           cuamp5
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7050625
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.0000 0.02844(8) 0.2500 0.0344(5) Uani 1 d S . .
Cu2 Cu -0.12826(10) -0.08938(5) 0.22681(8) 0.0332(4) Uani 1 d . . .
Cu3 Cu -0.2500 -0.2500 0.5000 0.0363(5) Uani 1 d S . .
N11 N -0.0072(8) 0.0998(4) 0.1555(6) 0.047(2) Uani 1 d . . .
C12 C -0.0989(9) 0.1355(5) 0.1167(7) 0.041(3) Uani 1 d . . .
N13 N -0.0969(7) 0.1884(4) 0.0721(5) 0.039(2) Uani 1 d . . .
C14 C 0.0101(10) 0.2055(5) 0.0706(7) 0.054(3) Uani 1 d . . .
H14A H 0.0176 0.2426 0.0418 0.065 Uiso 1 calc R . .
C15 C 0.1078(10) 0.1716(5) 0.1086(8) 0.056(3) Uani 1 d . . .
H15A H 0.1826 0.1848 0.1057 0.067 Uiso 1 calc R . .
C16 C 0.0999(10) 0.1190(5) 0.1510(7) 0.050(3) Uani 1 d . . .
H16A H 0.1692 0.0952 0.1778 0.060 Uiso 1 calc R . .
N17 N -0.2057(8) 0.1170(4) 0.1194(6) 0.063(3) Uani 1 d . . .
H17A H -0.2119 0.0824 0.1461 0.076 Uiso 1 calc R . .
H17B H -0.2692 0.1393 0.0944 0.076 Uiso 1 calc R . .
N21 N -0.2501(7) -0.1121(4) 0.1158(5) 0.033(2) Uani 1 d . . .
C22 C -0.2511(9) -0.1653(5) 0.0724(7) 0.036(3) Uani 1 d . . .
N23 N -0.3328(8) -0.1777(4) -0.0027(5) 0.036(2) Uani 1 d . . .
C24 C -0.4130(9) -0.1341(5) -0.0341(7) 0.042(3) Uani 1 d . . .
H24A H -0.4715 -0.1420 -0.0870 0.051 Uiso 1 calc R . .
C25 C -0.4176(9) -0.0779(5) 0.0049(7) 0.042(3) Uani 1 d . . .
H25A H -0.4760 -0.0472 -0.0196 0.051 Uiso 1 calc R . .
C26 C -0.3332(10) -0.0697(5) 0.0806(7) 0.045(3) Uani 1 d . . .
H26A H -0.3331 -0.0318 0.1101 0.054 Uiso 1 calc R . .
N27 N -0.1687(7) -0.2066(4) 0.1039(5) 0.041(2) Uani 1 d . . .
H27A H -0.1675 -0.2414 0.0762 0.049 Uiso 1 calc R . .
H27B H -0.1141 -0.1998 0.1529 0.049 Uiso 1 calc R . .
N31 N -0.2891(7) -0.1735(4) 0.3953(5) 0.043(2) Uani 1 d . . .
C32 C -0.2252(9) -0.1622(5) 0.3402(7) 0.040(3) Uani 1 d . . .
N33 N -0.2310(7) -0.1104(4) 0.2970(5) 0.040(2) Uani 1 d . . .
C34 C -0.3079(9) -0.0654(5) 0.3038(7) 0.046(3) Uani 1 d . . .
H34A H -0.3121 -0.0273 0.2740 0.055 Uiso 1 calc R . .
C35 C -0.3791(9) -0.0742(5) 0.3525(7) 0.050(3) Uani 1 d . . .
H35A H -0.4352 -0.0438 0.3563 0.060 Uiso 1 calc R . .
C36 C -0.3650(9) -0.1292(5) 0.3955(7) 0.048(3) Uani 1 d . . .
H36A H -0.4151 -0.1361 0.4289 0.058 Uiso 1 calc R . .
N37 N -0.1510(8) -0.2072(4) 0.3359(6) 0.052(3) Uani 1 d . . .
H37A H -0.1054 -0.2025 0.3041 0.062 Uiso 1 calc R . .
H37B H -0.1474 -0.2418 0.3650 0.062 Uiso 1 calc R . .
O1 O -0.0070(6) -0.0607(3) 0.1773(4) 0.0345(16) Uani 1 d . . .
C1 C -0.0151(10) -0.0589(5) 0.0918(7) 0.051(3) Uani 1 d . . .
H1A H -0.0175 -0.1015 0.0702 0.076 Uiso 1 calc R . .
H1B H 0.0541 -0.0371 0.0857 0.076 Uiso 1 calc R . .
H1C H -0.0875 -0.0367 0.0597 0.076 Uiso 1 calc R . .
F1 F -0.1662(4) 0.0171(2) 0.2205(3) 0.0369(14) Uani 1 d . . .
F2 F 0.0000 -0.1804(3) 0.2500 0.0311(18) Uani 1 d S . .
F3 F -0.1461(4) -0.2919(2) 0.4560(3) 0.0376(14) Uani 1 d . . .
B1 B 0.4722(13) 0.0860(4) 0.2449(9) 0.13(3) Uani 0.50 d PG A -1
F11 F 0.466(2) 0.0553(9) 0.3145(9) 0.104(10) Uani 0.50 d PG A -1
F12 F 0.5583(12) 0.0597(14) 0.2183(16) 0.145(15) Uani 0.50 d PG A -1
F13 F 0.499(3) 0.1470(5) 0.2641(16) 0.203(14) Uani 0.50 d PG A -1
F14 F 0.3660(11) 0.0818(8) 0.1824(8) 0.081(5) Uani 0.50 d PG A -1
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'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 '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
F1 Cu1 F1 165.2(3) . 2 ?
F1 Cu1 N11 96.1(3) . . ?
F1 Cu1 N11 94.3(3) 2 . ?
F1 Cu1 N11 94.3(3) . 2 ?
F1 Cu1 N11 96.1(3) 2 2 ?
N11 Cu1 N11 91.0(5) . 2 ?
F1 Cu1 O1 83.5(2) . 2 ?
F1 Cu1 O1 84.0(2) 2 2 ?
N11 Cu1 O1 166.5(3) . 2 ?
N11 Cu1 O1 102.5(3) 2 2 ?
F1 Cu1 O1 84.0(2) . . ?
F1 Cu1 O1 83.5(2) 2 . ?
N11 Cu1 O1 102.5(3) . . ?
N11 Cu1 O1 166.5(3) 2 . ?
O1 Cu1 O1 63.9(3) 2 . ?
F1 Cu1 Cu2 52.76(16) . . ?
F1 Cu1 Cu2 112.47(17) 2 . ?
N11 Cu1 Cu2 127.9(3) . . ?
N11 Cu1 Cu2 127.0(2) 2 . ?
O1 Cu1 Cu2 42.56(17) 2 . ?
O1 Cu1 Cu2 42.70(15) . . ?
F1 Cu1 Cu2 112.47(17) . 2 ?
F1 Cu1 Cu2 52.76(16) 2 2 ?
N11 Cu1 Cu2 127.0(2) . 2 ?
N11 Cu1 Cu2 127.9(3) 2 2 ?
O1 Cu1 Cu2 42.70(15) 2 2 ?
O1 Cu1 Cu2 42.56(17) . 2 ?
Cu2 Cu1 Cu2 59.71(7) . 2 ?
O1 Cu2 O1 74.3(3) 2 . ?
O1 Cu2 N33 94.9(3) 2 . ?
O1 Cu2 N33 169.0(3) . . ?
O1 Cu2 N21 169.6(3) 2 . ?
O1 Cu2 N21 95.5(3) . . ?
N33 Cu2 N21 95.3(3) . . ?
O1 Cu2 F1 80.0(2) 2 . ?
O1 Cu2 F1 80.4(2) . . ?
N33 Cu2 F1 95.8(3) . . ?
N21 Cu2 F1 97.1(3) . . ?
O1 Cu2 Cu2 42.86(17) 2 2 ?
O1 Cu2 Cu2 42.71(19) . 2 ?
N33 Cu2 Cu2 129.2(3) . 2 ?
N21 Cu2 Cu2 129.2(2) . 2 ?
F1 Cu2 Cu2 100.65(12) . 2 ?
O1 Cu2 Cu1 50.55(18) 2 . ?
O1 Cu2 Cu1 50.54(18) . . ?
N33 Cu2 Cu1 120.7(2) . . ?
N21 Cu2 Cu1 121.6(2) . . ?
F1 Cu2 Cu1 40.50(12) . . ?
Cu2 Cu2 Cu1 60.14(3) 2 . ?
F3 Cu3 F3 180.0 7_446 . ?
F3 Cu3 N13 91.8(3) 7_446 6_556 ?
F3 Cu3 N13 88.2(3) . 6_556 ?
F3 Cu3 N13 88.2(3) 7_446 4_445 ?
F3 Cu3 N13 91.8(3) . 4_445 ?
N13 Cu3 N13 180.0 6_556 4_445 ?
F3 Cu3 N31 87.7(2) 7_446 . ?
F3 Cu3 N31 92.3(2) . . ?
N13 Cu3 N31 85.6(3) 6_556 . ?
N13 Cu3 N31 94.4(3) 4_445 . ?
F3 Cu3 N31 92.3(2) 7_446 7_446 ?
F3 Cu3 N31 87.7(2) . 7_446 ?
N13 Cu3 N31 94.4(3) 6_556 7_446 ?
N13 Cu3 N31 85.6(3) 4_445 7_446 ?
N31 Cu3 N31 180.000(1) . 7_446 ?
C12 N11 C16 115.9(9) . . ?
C12 N11 Cu1 126.7(7) . . ?
C16 N11 Cu1 115.5(7) . . ?
N11 C12 N17 116.8(10) . . ?
N11 C12 N13 126.6(10) . . ?
N17 C12 N13 116.6(10) . . ?
C14 N13 C12 115.1(9) . . ?
C14 N13 Cu3 116.1(7) . 4_455 ?
C12 N13 Cu3 128.8(7) . 4_455 ?
N13 C14 C15 121.9(10) . . ?
N13 C14 H14A 119.0 . . ?
C15 C14 H14A 119.0 . . ?
C14 C15 C16 120.3(11) . . ?
C14 C15 H15A 119.8 . . ?
C16 C15 H15A 119.8 . . ?
C15 C16 N11 120.2(11) . . ?
C15 C16 H16A 119.9 . . ?
N11 C16 H16A 119.9 . . ?
C12 N17 H17A 120.0 . . ?
C12 N17 H17B 120.0 . . ?
H17A N17 H17B 120.0 . . ?
C26 N21 C22 117.4(9) . . ?
C26 N21 Cu2 117.1(7) . . ?
C22 N21 Cu2 125.4(7) . . ?
N27 C22 N23 118.0(9) . . ?
N27 C22 N21 118.8(10) . . ?
N23 C22 N21 123.2(10) . . ?
C24 N23 C22 116.5(9) . . ?
N23 C24 C25 124.3(11) . . ?
N23 C24 H24A 117.9 . . ?
C25 C24 H24A 117.9 . . ?
C26 C25 C24 115.2(10) . . ?
C26 C25 H25A 122.4 . . ?
C24 C25 H25A 122.4 . . ?
N21 C26 C25 123.3(10) . . ?
N21 C26 H26A 118.4 . . ?
C25 C26 H26A 118.4 . . ?
C22 N27 H27A 120.0 . . ?
C22 N27 H27B 120.0 . . ?
H27A N27 H27B 120.0 . . ?
C36 N31 C32 113.5(9) . . ?
C36 N31 Cu3 118.6(7) . . ?
C32 N31 Cu3 126.8(7) . . ?
N33 C32 N37 120.3(9) . . ?
N33 C32 N31 124.6(9) . . ?
N37 C32 N31 115.1(9) . . ?
C32 N33 C34 118.2(8) . . ?
C32 N33 Cu2 125.4(7) . . ?
C34 N33 Cu2 116.3(7) . . ?
N33 C34 C35 121.0(10) . . ?
N33 C34 H34A 119.5 . . ?
C35 C34 H34A 119.5 . . ?
C36 C35 C34 116.1(10) . . ?
C36 C35 H35A 121.9 . . ?
C34 C35 H35A 121.9 . . ?
N31 C36 C35 126.4(9) . . ?
N31 C36 H36A 116.8 . . ?
C35 C36 H36A 116.8 . . ?
C32 N37 H37A 120.0 . . ?
C32 N37 H37B 120.0 . . ?
H37A N37 H37B 120.0 . . ?
C1 O1 Cu2 127.6(6) . 2 ?
C1 O1 Cu2 127.9(6) . . ?
Cu2 O1 Cu2 94.4(3) 2 . ?
C1 O1 Cu1 120.4(6) . . ?
Cu2 O1 Cu1 86.9(2) 2 . ?
Cu2 O1 Cu1 86.8(2) . . ?
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
Cu1 F1 Cu2 86.7(2) . . ?
F11 B1 F14 109.5 . . ?
F11 B1 F13 109.5 . . ?
F14 B1 F13 109.5 . . ?
F11 B1 F12 109.5 . . ?
F14 B1 F12 109.5 . . ?
F13 B1 F12 109.5 . . ?
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
Cu1 F1 1.894(5) . ?
Cu1 F1 1.894(5) 2 ?
Cu1 N11 2.181(9) . ?
Cu1 N11 2.181(9) 2 ?
Cu1 O1 2.252(7) 2 ?
Cu1 O1 2.252(7) . ?
Cu1 Cu2 2.912(2) . ?
Cu1 Cu2 2.912(2) 2 ?
Cu2 O1 1.972(7) 2 ?
Cu2 O1 1.978(6) . ?
Cu2 N33 1.999(8) . ?
Cu2 N21 2.016(8) . ?
Cu2 F1 2.322(5) . ?
Cu2 Cu2 2.899(3) 2 ?
Cu3 F3 1.860(5) 7_446 ?
Cu3 F3 1.860(5) . ?
Cu3 N13 2.262(9) 6_556 ?
Cu3 N13 2.262(9) 4_445 ?
Cu3 N31 2.335(8) . ?
Cu3 N31 2.335(8) 7_446 ?
N11 C12 1.322(13) . ?
N11 C16 1.364(12) . ?
C12 N17 1.346(12) . ?
C12 N13 1.360(13) . ?
N13 C14 1.333(12) . ?
N13 Cu3 2.262(9) 4_455 ?
C14 C15 1.345(14) . ?
C14 H14A 0.9500 . ?
C15 C16 1.352(14) . ?
C15 H15A 0.9500 . ?
C16 H16A 0.9500 . ?
N17 H17A 0.8800 . ?
N17 H17B 0.8800 . ?
N21 C26 1.333(12) . ?
N21 C22 1.349(12) . ?
C22 N27 1.302(12) . ?
C22 N23 1.347(12) . ?
N23 C24 1.318(12) . ?
C24 C25 1.379(14) . ?
C24 H24A 0.9500 . ?
C25 C26 1.353(14) . ?
C25 H25A 0.9500 . ?
C26 H26A 0.9500 . ?
N27 H27A 0.8800 . ?
N27 H27B 0.8800 . ?
N31 C36 1.312(12) . ?
N31 C32 1.390(11) . ?
C32 N33 1.315(12) . ?
C32 N37 1.325(12) . ?
N33 C34 1.358(12) . ?
C34 C35 1.364(13) . ?
C34 H34A 0.9500 . ?
C35 C36 1.362(14) . ?
C35 H35A 0.9500 . ?
C36 H36A 0.9500 . ?
N37 H37A 0.8800 . ?
N37 H37B 0.8800 . ?
O1 C1 1.403(11) . ?
O1 Cu2 1.972(7) 2 ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
B1 F11 1.3603 . ?
B1 F14 1.3605 . ?
B1 F13 1.3607 . ?
B1 F12 1.3607 . ?
