#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:29:14 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179181 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/29/4312974.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_4312974
loop_
_publ_author_name
'John F. Berry'
'F. Albert Cotton'
'Peng Lei'
'Carlos A. Murillo'
_publ_section_title
;
 Further Structural and Magnetic Studies of Tricopper Dipyridylamido
 Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              377
_journal_page_last               382
_journal_paper_doi               10.1021/ic025957c
_journal_volume                  42
_journal_year                    2003
_chemical_compound_source        synthesis
_chemical_formula_structural     'Cu3(dpa)4Cl2 CH2Cl2'
_chemical_formula_sum            'C41 H34 Cl4 Cu3 N12'
_chemical_formula_weight         1027.22
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           34
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 -2n'
_symmetry_space_group_name_H-M   'P n n 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.952(11)
_cell_length_b                   14.113(12)
_cell_length_c                   11.430(9)
_cell_measurement_reflns_used    6897
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      54.769
_cell_measurement_theta_min      4.268
_cell_volume                     2089(3)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL v5.02 (Siemens, 1993)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measurement_device       'Bruker SMART 1000'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0171
_diffrn_reflns_av_sigmaI/netI    0.0202
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12201
_diffrn_reflns_theta_max         27.30
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    1.817
_exptl_absorpt_correction_T_max  0.63492
_exptl_absorpt_correction_T_min  0.51524
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1038
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.897
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.007(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.055
_refine_ls_goodness_of_fit_obs   1.072
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         4612
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.055
_refine_ls_restrained_S_obs      1.072
_refine_ls_R_factor_all          0.0297
_refine_ls_R_factor_obs          0.0268
_refine_ls_shift/esd_max         0.142
_refine_ls_shift/esd_mean        0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0387P)²+0.9959P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0701
_refine_ls_wR_factor_obs         0.0684
_reflns_number_observed          4273
_reflns_number_total             4612
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic025957c_s2.cif
_cod_data_source_block           xl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0387P)^2^+0.9959P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0387P)^2^+0.9959P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2089.2(30)
_cod_database_code               4312974
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x+1/2, -y+1/2, z+1/2'
'-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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Cu1 Cu 0.66469(2) 1.59131(2) -0.17663(3) 0.01671(7) Uani 1 d . .
Cu2 Cu 0.5000 1.5000 -0.17988(5) 0.01493(8) Uani 1 d S .
N1 N 0.6089(2) 1.62358(15) -0.0088(2) 0.0190(4) Uani 1 d . .
N2 N 0.5704(2) 1.6958(2) -0.2442(2) 0.0228(5) Uani 1 d . .
N3 N 0.7245(2) 1.46762(15) -0.1102(2) 0.0183(4) Uani 1 d . .
N4 N 0.6755(2) 1.5300(2) -0.3466(2) 0.0203(4) Uani 1 d . .
N5 N 0.5521(2) 1.4145(2) -0.3041(2) 0.0182(5) Uani 1 d . .
N6 N 0.5601(2) 1.4164(2) -0.0581(2) 0.0184(5) Uani 1 d . .
C1 C 0.5068(2) 1.6197(2) 0.0236(2) 0.0194(5) Uani 1 d . .
C2 C 0.4786(2) 1.6462(2) 0.1404(2) 0.0261(6) Uani 1 d . .
H2 H 0.4097(2) 1.6435(2) 0.1632(2) 0.031 Uiso 1 calc R .
C3 C 0.5522(2) 1.6754(2) 0.2186(3) 0.0336(7) Uani 1 d . .
H3 H 0.5331(2) 1.6939(2) 0.2936(3) 0.040 Uiso 1 calc R .
C4 C 0.6559(2) 1.6774(2) 0.1853(3) 0.0317(7) Uani 1 d . .
H4 H 0.7069(2) 1.6961(2) 0.2377(3) 0.038 Uiso 1 calc R .
C5 C 0.6808(2) 1.6508(2) 0.0717(3) 0.0257(6) Uani 1 d . .
H5 H 0.7498(2) 1.6516(2) 0.0494(3) 0.031 Uiso 1 calc R .
C6 C 0.4804(2) 1.6781(2) -0.3040(2) 0.0214(5) Uani 1 d . .
C7 C 0.4240(2) 1.7544(2) -0.3537(3) 0.0305(6) Uani 1 d . .
H7 H 0.3646(2) 1.7425(2) -0.3969(3) 0.037 Uiso 1 calc R .
C8 C 0.4578(2) 1.8467(2) -0.3376(4) 0.0418(8) Uani 1 d . .
H8 H 0.4213(2) 1.8969(2) -0.3702(4) 0.050 Uiso 1 calc R .
C9 C 0.5469(3) 1.8641(2) -0.2722(4) 0.0504(10) Uani 1 d . .
H9 H 0.5698(3) 1.9255(2) -0.2588(4) 0.061 Uiso 1 calc R .
C10 C 0.5996(2) 1.7873(2) -0.2283(3) 0.0362(7) Uani 1 d . .
H10 H 0.6590(2) 1.7988(2) -0.1849(3) 0.043 Uiso 1 calc R .
C11 C 0.8275(2) 1.4524(2) -0.1208(2) 0.0238(6) Uani 1 d . .
H11 H 0.8670(2) 1.4986(2) -0.1577(2) 0.029 Uiso 1 calc R .
C12 C 0.8773(2) 1.3725(2) -0.0801(3) 0.0296(6) Uani 1 d . .
H12 H 0.9484(2) 1.3655(2) -0.0878(3) 0.035 Uiso 1 calc R .
C13 C 0.8170(2) 1.3023(2) -0.0269(3) 0.0307(6) Uani 1 d . .
H13 H 0.8478(2) 1.2475(2) 0.0020(3) 0.037 Uiso 1 calc R .
C14 C 0.7115(2) 1.3146(2) -0.0174(3) 0.0269(6) Uani 1 d . .
H14 H 0.6712(2) 1.2671(2) 0.0157(3) 0.032 Uiso 1 calc R .
C15 C 0.6642(2) 1.3994(2) -0.0581(2) 0.0186(5) Uani 1 d . .
C16 C 0.7402(2) 1.5741(2) -0.4231(3) 0.0255(6) Uani 1 d . .
H16 H 0.7772(2) 1.6264(2) -0.3970(3) 0.031 Uiso 1 calc R .
C17 C 0.7537(3) 1.5450(2) -0.5379(3) 0.0348(7) Uani 1 d . .
H17 H 0.8001(3) 1.5761(2) -0.5868(3) 0.042 Uiso 1 calc R .
C18 C 0.6965(3) 1.4681(2) -0.5784(2) 0.0360(7) Uani 1 d . .
H18 H 0.7027(3) 1.4482(2) -0.6556(2) 0.043 Uiso 1 calc R .
C19 C 0.6298(2) 1.4214(2) -0.5023(2) 0.0284(6) Uani 1 d . .
H19 H 0.5917(2) 1.3697(2) -0.5284(2) 0.034 Uiso 1 calc R .
C20 C 0.6201(2) 1.4529(2) -0.3839(2) 0.0208(5) Uani 1 d . .
Cl1 Cl 0.82696(4) 1.68556(4) -0.17375(8) 0.02565(12) Uani 1 d . .
Cl1S Cl 1.0144(2) 1.61220(14) -0.5079(2) 0.0493(4) Uiso 0.50 d P .
Cl2S Cl 1.0309(2) 1.5739(2) -0.4003(2) 0.0681(7) Uiso 0.50 d P .
C1S C 1.0119(4) 1.5452(3) -0.3716(4) 0.0086(8) Uiso 0.50 d P .
H1SA H 0.9458(4) 1.5741(3) -0.3538(4) 0.010 Uiso 0.50 calc PR .
H1SB H 1.0512(4) 1.5507(3) -0.2997(4) 0.010 Uiso 0.50 calc PR .
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'
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'
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
N3 Cu1 N2 165.41(9) . . y
N3 Cu1 N1 88.66(9) . . y
N2 Cu1 N1 89.04(10) . . y
N3 Cu1 N4 88.11(9) . . y
N2 Cu1 N4 89.30(10) . . y
N1 Cu1 N4 160.62(8) . . y
N3 Cu1 Cl1 97.51(8) . . y
N2 Cu1 Cl1 97.08(9) . . y
N1 Cu1 Cl1 99.35(7) . . y
N4 Cu1 Cl1 100.01(7) . . y
N3 Cu1 Cu2 83.63(8) . . y
N2 Cu1 Cu2 81.78(8) . . y
N1 Cu1 Cu2 80.30(6) . . y
N4 Cu1 Cu2 80.36(6) . . y
Cl1 Cu1 Cu2 178.80(2) . . y
N5 Cu2 N5 88.5(2) 2_685 . y
N5 Cu2 N6 176.80(11) 2_685 . y
N5 Cu2 N6 90.40(10) . . y
N5 Cu2 N6 90.40(10) 2_685 2_685 y
N5 Cu2 N6 176.80(11) . 2_685 ?
N6 Cu2 N6 90.9(2) . 2_685 ?
N5 Cu2 Cu1 89.29(8) 2_685 . ?
N5 Cu2 Cu1 91.94(8) . . ?
N6 Cu2 Cu1 87.76(8) . . ?
N6 Cu2 Cu1 91.04(8) 2_685 . ?
N5 Cu2 Cu1 91.94(8) 2_685 2_685 ?
N5 Cu2 Cu1 89.29(8) . 2_685 ?
N6 Cu2 Cu1 91.04(8) . 2_685 ?
N6 Cu2 Cu1 87.76(8) 2_685 2_685 ?
Cu1 Cu2 Cu1 178.29(3) . 2_685 ?
C5 N1 C1 119.1(2) . . ?
C5 N1 Cu1 116.3(2) . . ?
C1 N1 Cu1 124.6(2) . . ?
C10 N2 C6 118.4(2) . . ?
C10 N2 Cu1 117.7(2) . . ?
C6 N2 Cu1 124.0(2) . . ?
C11 N3 C15 119.1(2) . . ?
C11 N3 Cu1 118.2(2) . . ?
C15 N3 Cu1 122.7(2) . . ?
C16 N4 C20 119.0(2) . . ?
C16 N4 Cu1 116.1(2) . . ?
C20 N4 Cu1 124.9(2) . . ?
C6 N5 C20 124.8(2) 2_685 . ?
C6 N5 Cu2 118.3(2) 2_685 . ?
C20 N5 Cu2 116.9(2) . . ?
C15 N6 C1 123.8(2) . 2_685 ?
C15 N6 Cu2 119.4(2) . . ?
C1 N6 Cu2 116.7(2) 2_685 . ?
N6 C1 N1 116.1(2) 2_685 . ?
N6 C1 C2 124.7(2) 2_685 . ?
N1 C1 C2 119.1(2) . . ?
C3 C2 C1 120.5(3) . . ?
C2 C3 C4 119.8(3) . . ?
C5 C4 C3 118.2(3) . . ?
N1 C5 C4 123.2(3) . . ?
N5 C6 N2 115.7(2) 2_685 . ?
N5 C6 C7 124.4(3) 2_685 . ?
N2 C6 C7 119.8(2) . . ?
C8 C7 C6 119.8(3) . . ?
C7 C8 C9 119.8(3) . . ?
C10 C9 C8 117.9(3) . . ?
N2 C10 C9 124.2(3) . . ?
N3 C11 C12 124.0(3) . . ?
C11 C12 C13 117.6(3) . . ?
C14 C13 C12 119.8(3) . . ?
C13 C14 C15 120.4(3) . . ?
N6 C15 N3 115.9(2) . . ?
N6 C15 C14 124.9(2) . . ?
N3 C15 C14 119.0(2) . . ?
N4 C16 C17 123.4(3) . . ?
C16 C17 C18 118.5(3) . . ?
C17 C18 C19 119.5(3) . . ?
C18 C19 C20 119.9(3) . . ?
N4 C20 N5 116.1(2) . . ?
N4 C20 C19 119.7(2) . . ?
N5 C20 C19 124.1(3) . . ?
Cl2S Cl1S C1S 12.6(2) . . ?
C1S Cl2S Cl1S 136.6(6) . . ?
C1S Cl2S C1S 27.0(5) . 2_785 ?
Cl1S Cl2S C1S 119.1(3) . 2_785 ?
C1S Cl2S Cl2S 36.0(6) . 2_785 ?
Cl1S Cl2S Cl2S 108.3(2) . 2_785 ?
C1S Cl2S Cl2S 10.8(2) 2_785 2_785 ?
Cl2S C1S C1S 141.6(6) . 2_785 ?
Cl2S C1S Cl2S 133.2(7) . 2_785 ?
C1S C1S Cl2S 11.5(2) 2_785 2_785 ?
Cl2S C1S Cl1S 30.9(5) . . ?
C1S C1S Cl1S 120.6(2) 2_785 . ?
Cl2S C1S Cl1S 109.5(3) 2_785 . ?
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 N3 2.055(2) . y
Cu1 N2 2.064(2) . y
Cu1 N1 2.100(3) . y
Cu1 N4 2.131(3) . y
Cu1 Cl1 2.487(2) . y
Cu1 Cu2 2.492(2) . y
Cu2 N5 1.981(3) 2_685 y
Cu2 N5 1.981(3) . y
Cu2 N6 1.984(3) . y
Cu2 N6 1.984(3) 2_685 y
Cu2 Cu1 2.492(2) 2_685 y
N1 C5 1.364(3) . ?
N1 C1 1.374(3) . ?
N2 C10 1.359(4) . ?
N2 C6 1.374(4) . ?
N3 C11 1.357(3) . ?
N3 C15 1.375(3) . ?
N4 C16 1.362(3) . ?
N4 C20 1.372(4) . ?
N5 C6 1.374(4) 2_685 ?
N5 C20 1.379(4) . ?
N6 C15 1.369(4) . ?
N6 C1 1.373(4) 2_685 ?
C1 N6 1.373(4) 2_685 ?
C1 C2 1.434(4) . ?
C2 C3 1.371(4) . ?
C3 C4 1.397(4) . ?
C4 C5 1.390(4) . ?
C6 N5 1.374(4) 2_685 ?
C6 C7 1.419(4) . ?
C7 C8 1.386(4) . ?
C8 C9 1.396(5) . ?
C9 C10 1.375(4) . ?
C11 C12 1.379(4) . ?
C12 C13 1.402(4) . ?
C13 C14 1.381(4) . ?
C14 C15 1.424(4) . ?
C16 C17 1.386(4) . ?
C17 C18 1.394(5) . ?
C18 C19 1.391(4) . ?
C19 C20 1.430(4) . ?
Cl1S Cl2S 1.361(3) . ?
Cl1S C1S 1.823(5) . ?
Cl2S C1S 0.576(5) . ?
Cl2S C1S 1.800(6) 2_785 ?
Cl2S Cl2S 2.235(6) 2_785 ?
C1S C1S 1.313(9) 2_785 ?
C1S Cl2S 1.800(6) 2_785 ?
