#------------------------------------------------------------------------------
#$Date: 2018-09-07 16:01:56 +0300 (Fri, 07 Sep 2018) $
#$Revision: 210535 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/11/34/7113489.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_7113489
loop_
_publ_author_name
'Gheorghe, Ruxandra'
'Andruh, Marius'
'Costes, Jean-Pierre'
'Donnadieu, Bruno'
_publ_section_title
;
 A rational synthetic route leading to 3d--3d'--4f heterospin systems:
 self-assembly processes involving heterobinuclear 3d--4f complexes and
 hexacyanometallates
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   22
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              2778
_journal_page_last               2779
_journal_paper_doi               10.1039/b310082k
_journal_year                    2003
_chemical_formula_sum            'C25 H17 Co Cu Gd N8 O10.5'
_chemical_formula_weight         877.19
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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            4
_cell_length_a                   12.945(3)
_cell_length_b                   15.010(3)
_cell_length_c                   16.955(3)
_cell_measurement_temperature    180(2)
_cell_volume                     3294.4(12)
_computing_cell_refinement
'Crysalis Red, Vers 1.170 14 release 25 11 2002'
_computing_data_collection
'Crysalis Red, Vers 1.170 14 release 25 11 2002'
_computing_data_reduction
'Crysalis Red, Vers 1.170 14 release 25 11 2002'
_computing_molecular_graphics    'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1992)'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'KappaCCD Xcalibur'
_diffrn_measurement_method       'omega, phi scan'
_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  0.1117
_diffrn_reflns_av_sigmaI/netI    0.0755
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            25146
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.14
_diffrn_standards_decay_%        0.1
_diffrn_standards_interval_time  27
_exptl_absorpt_coefficient_mu    3.192
_exptl_absorpt_correction_T_max  0.666
_exptl_absorpt_correction_T_min  0.197
_exptl_absorpt_correction_type   refdelf
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.769
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1708
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.366
_refine_diff_density_min         -1.002
_refine_diff_density_rms         0.184
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.024(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         6719
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0535
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0808P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1309
_refine_ls_wR_factor_ref         0.1385
_reflns_number_gt                5717
_reflns_number_total             6719
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7104902
_cod_data_source_file            b310082k.txt
_cod_data_source_block           (2)
_cod_original_cell_volume        3294.3(11)
_cod_original_sg_symbol_H-M      ' P 21 21 21'
_cod_original_formula_sum        'C25 H17 Co Cu Gd N8 O10.50'
_cod_database_code               7113489
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -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
Gd1 Gd 0.91311(3) 0.59808(3) 0.91271(2) 0.02196(12) Uani 1 1 d .
Cu1 Cu 0.70484(6) 0.44838(7) 0.90901(7) 0.0238(2) Uani 1 1 d .
Co1 Co 1.33530(7) 0.60032(7) 0.90845(6) 0.0200(2) Uani 1 1 d .
N1 N 0.6262(5) 0.3909(5) 0.9941(4) 0.0255(15) Uani 1 1 d .
N2 N 0.6329(5) 0.3863(5) 0.8219(4) 0.0219(15) Uani 1 1 d .
N3 N 1.1027(5) 0.6284(5) 0.9173(5) 0.0299(15) Uani 1 1 d .
N4 N 1.2834(6) 0.4255(6) 0.8252(5) 0.039(2) Uani 1 1 d .
N5 N 1.3439(7) 0.6725(6) 0.7413(5) 0.042(2) Uani 1 1 d .
N6 N 1.5679(5) 0.5669(5) 0.9007(4) 0.0285(16) Uani 1 1 d .
N7 N 1.3883(6) 0.7727(5) 0.9927(5) 0.0349(18) Uani 1 1 d .
N8 N 1.3152(6) 0.5170(5) 1.0698(5) 0.0356(19) Uani 1 1 d .
O1 O 0.7970(4) 0.5077(4) 0.9864(3) 0.0236(13) Uani 1 1 d .
O2 O 0.8044(4) 0.5031(4) 0.8367(3) 0.0247(13) Uani 1 1 d .
O3 O 0.9691(4) 0.5604(4) 1.0536(4) 0.0280(13) Uani 1 1 d .
O4 O 0.9730(4) 0.5663(4) 0.7714(4) 0.0284(13) Uani 1 1 d .
O5 O 0.9900(4) 0.4513(4) 0.9131(4) 0.0324(13) Uani 1 1 d .
C1 C 0.5200(7) 0.3580(7) 0.9811(5) 0.031(2) Uani 1 1 d .
H1A H 0.4724 0.4093 0.9766 0.037 Uiso 1 1 calc R
H1B H 0.4982 0.3220 1.0272 0.037 Uiso 1 1 calc R
C2 C 0.5125(6) 0.3019(6) 0.9074(6) 0.0304(18) Uani 1 1 d .
H2A H 0.5652 0.2543 0.9101 0.036 Uiso 1 1 calc R
H2B H 0.4438 0.2729 0.9063 0.036 Uiso 1 1 calc R
C3 C 0.5271(7) 0.3529(7) 0.8319(6) 0.033(2) Uani 1 1 d .
H3A H 0.5097 0.3136 0.7869 0.039 Uiso 1 1 calc R
H3B H 0.4786 0.4038 0.8311 0.039 Uiso 1 1 calc R
C4 C 0.6730(6) 0.3751(6) 0.7544(5) 0.0257(19) Uani 1 1 d .
H4 H 0.6322 0.3430 0.7175 0.031 Uiso 1 1 calc R
C5 C 0.7729(6) 0.4047(6) 0.7260(5) 0.0247(16) Uani 1 1 d .
C6 C 0.8067(7) 0.3721(7) 0.6513(5) 0.033(2) Uani 1 1 d .
H6 H 0.7663 0.3292 0.6239 0.039 Uiso 1 1 calc R
C7 C 0.8970(7) 0.4022(7) 0.6189(5) 0.035(2) Uani 1 1 d .
H7 H 0.9199 0.3787 0.5699 0.042 Uiso 1 1 calc R
C8 C 0.9561(7) 0.4675(7) 0.6574(5) 0.030(2) Uani 1 1 d .
H8 H 1.0178 0.4893 0.6340 0.036 Uiso 1 1 calc R
C9 C 0.9232(6) 0.5003(6) 0.7304(5) 0.0243(17) Uani 1 1 d .
C10 C 0.8319(6) 0.4685(5) 0.7663(5) 0.0218(16) Uani 1 1 d .
C11 C 0.8249(6) 0.4679(6) 1.0547(5) 0.0249(17) Uani 1 1 d .
C12 C 0.9165(6) 0.4925(5) 1.0914(5) 0.0265(16) Uani 1 1 d .
C13 C 0.9512(7) 0.4514(7) 1.1602(5) 0.032(2) Uani 1 1 d .
H13 H 1.0162 0.4670 1.1822 0.038 Uiso 1 1 calc R
C14 C 0.8911(8) 0.3888(8) 1.1954(5) 0.043(3) Uani 1 1 d .
H14 H 0.9135 0.3613 1.2428 0.052 Uiso 1 1 calc R
C15 C 0.7976(8) 0.3650(7) 1.1625(6) 0.034(2) Uani 1 1 d .
H15 H 0.7552 0.3224 1.1883 0.041 Uiso 1 1 calc R
C16 C 0.7647(5) 0.4025(6) 1.0921(5) 0.0257(16) Uani 1 1 d .
C17 C 0.6642(7) 0.3737(6) 1.0624(6) 0.031(2) Uani 1 1 d .
H17 H 0.6230 0.3388 1.0970 0.037 Uiso 1 1 calc R
C18 C 1.0541(6) 0.6000(7) 1.0951(6) 0.037(2) Uani 1 1 d .
H18A H 1.0345 0.6100 1.1503 0.055 Uiso 1 1 calc R
H18B H 1.0719 0.6571 1.0705 0.055 Uiso 1 1 calc R
H18C H 1.1139 0.5601 1.0930 0.055 Uiso 1 1 calc R
C19 C 1.0674(6) 0.5988(8) 0.7330(5) 0.035(2) Uani 1 1 d .
C20 C 1.1903(5) 0.6218(5) 0.9140(6) 0.0229(15) Uani 1 1 d .
C21 C 1.3039(6) 0.4904(6) 0.8572(6) 0.0284(19) Uani 1 1 d .
C22 C 1.3395(7) 0.6491(7) 0.8057(6) 0.034(2) Uani 1 1 d .
C23 C 1.4821(5) 0.5823(5) 0.9047(4) 0.0181(15) Uani 1 1 d .
C24 C 1.3659(6) 0.7094(6) 0.9579(5) 0.0276(18) Uani 1 1 d .
C25 C 1.3249(6) 0.5478(6) 1.0092(5) 0.0236(17) Uani 1 1 d .
O1W O 0.7502(5) 0.6713(5) 0.8806(4) 0.0399(17) Uani 1 1 d .
O3W O 0.9470(5) 0.7377(4) 0.8381(4) 0.0337(15) Uani 1 1 d .
O4W O 0.2755(5) 0.6588(5) 1.1819(4) 0.0397(16) Uani 1 1 d .
O5W O 0.2551(5) 0.6611(5) 1.5936(5) 0.0450(16) Uani 1 1 d .
O6W O 0.1515(5) 0.3406(5) 1.9451(5) 0.0503(19) Uani 1 1 d .
O7W O 0.8529(8) 0.3132(7) 1.9159(14) 0.065(6) Uani 0.50 1 d P
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'
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'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 '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
O1 Gd1 O2 64.49(17) . .
O1 Gd1 O5 74.9(2) . .
O2 Gd1 O5 72.5(2) . .
O1 Gd1 O1W 80.1(2) . .
O2 Gd1 O1W 68.8(2) . .
O5 Gd1 O1W 140.1(2) . .
O1 Gd1 O3W 149.21(19) . .
O2 Gd1 O3W 109.5(2) . .
O5 Gd1 O3W 134.2(2) . .
O1W Gd1 O3W 70.1(2) . .
O1 Gd1 N3 135.1(2) . .
O2 Gd1 N3 135.0(2) . .
O5 Gd1 N3 76.2(2) . .
O1W Gd1 N3 140.8(2) . .
O3W Gd1 N3 71.9(2) . .
O1 Gd1 N7 91.4(2) . 4_467
O2 Gd1 N7 136.4(2) . 4_467
O5 Gd1 N7 138.3(2) . 4_467
O1W Gd1 N7 71.8(2) . 4_467
O3W Gd1 N7 72.5(2) . 4_467
N3 Gd1 N7 88.0(2) . 4_467
O1 Gd1 O3 64.09(19) . .
O2 Gd1 O3 122.7(2) . .
O5 Gd1 O3 71.3(2) . .
O1W Gd1 O3 123.5(2) . .
O3W Gd1 O3 127.7(2) . .
N3 Gd1 O3 74.5(2) . .
N7 Gd1 O3 67.4(2) 4_467 .
O1 Gd1 O4 125.15(19) . .
O2 Gd1 O4 63.99(18) . .
O5 Gd1 O4 73.0(2) . .
O1W Gd1 O4 97.9(2) . .
O3W Gd1 O4 68.2(2) . .
N3 Gd1 O4 76.5(2) . .
N7 Gd1 O4 140.5(2) 4_467 .
O3 Gd1 O4 138.20(17) . .
O1 Gd1 Cu1 32.76(14) . .
O2 Gd1 Cu1 32.15(14) . .
O5 Gd1 Cu1 74.52(13) . .
O1W Gd1 Cu1 67.69(16) . .
O3W Gd1 Cu1 131.74(14) . .
N3 Gd1 Cu1 150.68(17) . .
N7 Gd1 Cu1 113.78(17) 4_467 .
O3 Gd1 Cu1 95.32(14) . .
O4 Gd1 Cu1 95.53(13) . .
O2 Cu1 N1 169.8(3) . .
O2 Cu1 N2 92.3(3) . .
N1 Cu1 N2 95.6(3) . .
O2 Cu1 O1 80.2(2) . .
N1 Cu1 O1 91.4(3) . .
N2 Cu1 O1 171.0(3) . .
O2 Cu1 Gd1 40.31(17) . .
N1 Cu1 Gd1 131.8(2) . .
N2 Cu1 Gd1 132.6(2) . .
O1 Cu1 Gd1 40.45(17) . .
C24 Co1 C25 88.6(4) . .
C24 Co1 C22 93.9(4) . .
C25 Co1 C22 176.9(4) . .
C24 Co1 C20 92.2(3) . .
C25 Co1 C20 87.5(4) . .
C22 Co1 C20 90.5(4) . .
C24 Co1 C21 179.3(4) . .
C25 Co1 C21 92.0(4) . .
C22 Co1 C21 85.5(4) . .
C20 Co1 C21 87.7(3) . .
C24 Co1 C23 85.9(3) . .
C25 Co1 C23 92.4(3) . .
C22 Co1 C23 89.8(3) . .
C20 Co1 C23 178.1(4) . .
C21 Co1 C23 94.2(3) . .
C17 N1 C1 115.1(8) . .
C17 N1 Cu1 123.5(6) . .
C1 N1 Cu1 121.3(6) . .
C4 N2 C3 116.2(7) . .
C4 N2 Cu1 122.9(6) . .
C3 N2 Cu1 121.0(6) . .
C20 N3 Gd1 163.9(6) . .
C24 N7 Gd1 169.5(7) . 4_567
C11 O1 Cu1 121.9(5) . .
C11 O1 Gd1 122.2(5) . .
Cu1 O1 Gd1 106.8(3) . .
C10 O2 Cu1 124.4(5) . .
C10 O2 Gd1 123.6(5) . .
Cu1 O2 Gd1 107.5(2) . .
C12 O3 C18 117.1(7) . .
C12 O3 Gd1 117.1(5) . .
C18 O3 Gd1 125.7(6) . .
C9 O4 C19 114.0(7) . .
C9 O4 Gd1 117.8(5) . .
C19 O4 Gd1 127.2(5) . .
N1 C1 C2 111.7(7) . .
N1 C1 H1A 109.3 . .
C2 C1 H1A 109.3 . .
N1 C1 H1B 109.3 . .
C2 C1 H1B 109.3 . .
H1A C1 H1B 107.9 . .
C3 C2 C1 114.4(7) . .
C3 C2 H2A 108.7 . .
C1 C2 H2A 108.7 . .
C3 C2 H2B 108.7 . .
C1 C2 H2B 108.7 . .
H2A C2 H2B 107.6 . .
N2 C3 C2 112.9(7) . .
N2 C3 H3A 109.0 . .
C2 C3 H3A 109.0 . .
N2 C3 H3B 109.0 . .
C2 C3 H3B 109.0 . .
H3A C3 H3B 107.8 . .
N2 C4 C5 128.7(8) . .
N2 C4 H4 115.7 . .
C5 C4 H4 115.7 . .
C10 C5 C6 120.0(8) . .
C10 C5 C4 122.2(8) . .
C6 C5 C4 117.6(8) . .
C7 C6 C5 120.3(9) . .
C7 C6 H6 119.8 . .
C5 C6 H6 119.8 . .
C6 C7 C8 120.6(8) . .
C6 C7 H7 119.7 . .
C8 C7 H7 119.7 . .
C9 C8 C7 119.4(8) . .
C9 C8 H8 120.3 . .
C7 C8 H8 120.3 . .
O4 C9 C8 124.1(8) . .
O4 C9 C10 114.8(7) . .
C8 C9 C10 121.2(8) . .
O2 C10 C5 123.4(7) . .
O2 C10 C9 118.1(7) . .
C5 C10 C9 118.5(8) . .
O1 C11 C12 119.6(8) . .
O1 C11 C16 123.2(8) . .
C12 C11 C16 117.2(8) . .
O3 C12 C11 114.1(8) . .
O3 C12 C13 123.7(8) . .
C11 C12 C13 122.2(8) . .
C14 C13 C12 119.3(8) . .
C14 C13 H13 120.4 . .
C12 C13 H13 120.4 . .
C13 C14 C15 120.3(9) . .
C13 C14 H14 119.9 . .
C15 C14 H14 119.9 . .
C14 C15 C16 120.8(9) . .
C14 C15 H15 119.6 . .
C16 C15 H15 119.6 . .
C15 C16 C11 120.1(8) . .
C15 C16 C17 116.7(8) . .
C11 C16 C17 123.1(8) . .
N1 C17 C16 126.3(9) . .
N1 C17 H17 116.8 . .
C16 C17 H17 116.8 . .
O3 C18 H18A 109.5 . .
O3 C18 H18B 109.5 . .
H18A C18 H18B 109.5 . .
O3 C18 H18C 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
N3 C20 Co1 175.2(7) . .
N4 C21 Co1 178.3(9) . .
N5 C22 Co1 174.9(9) . .
N6 C23 Co1 176.0(8) . .
N7 C24 Co1 174.8(8) . .
N8 C25 Co1 177.7(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Gd1 O1 2.379(6) .
Gd1 O2 2.381(6) .
Gd1 O5 2.418(6) .
Gd1 O1W 2.439(6) .
Gd1 O3W 2.488(7) .
Gd1 N3 2.498(6) .
Gd1 N7 2.537(8) 4_467
Gd1 O3 2.559(6) .
Gd1 O4 2.563(6) .
Gd1 Cu1 3.5102(11) .
Cu1 O2 1.959(6) .
Cu1 N1 1.966(7) .
Cu1 N2 1.979(7) .
Cu1 O1 1.984(6) .
Co1 C24 1.882(9) .
Co1 C25 1.885(9) .
Co1 C22 1.891(10) .
Co1 C20 1.907(7) .
Co1 C21 1.909(9) .
Co1 C23 1.921(7) .
N1 C17 1.285(11) .
N1 C1 1.477(11) .
N2 C4 1.268(11) .
N2 C3 1.469(11) .
N3 C20 1.139(10) .
N4 C21 1.146(12) .
N5 C22 1.148(12) .
N6 C23 1.136(9) .
N7 C24 1.155(11) .
N7 Gd1 2.537(8) 4_567
N8 C25 1.134(12) .
O1 C11 1.353(10) .
O2 C10 1.350(10) .
O3 C12 1.384(11) .
O3 C18 1.436(10) .
O4 C9 1.371(10) .
O4 C19 1.468(9) .
C1 C2 1.509(12) .
C1 H1A 0.9900 .
C1 H1B 0.9900 .
C2 C3 1.503(14) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C4 C5 1.450(11) .
C4 H4 0.9500 .
C5 C10 1.402(11) .
C5 C6 1.427(12) .
C6 C7 1.369(13) .
C6 H6 0.9500 .
C7 C8 1.404(14) .
C7 H7 0.9500 .
C8 C9 1.398(12) .
C8 H8 0.9500 .
C9 C10 1.412(11) .
C11 C12 1.389(12) .
C11 C16 1.404(12) .
C12 C13 1.394(13) .
C13 C14 1.358(15) .
C13 H13 0.9500 .
C14 C15 1.380(14) .
C14 H14 0.9500 .
C15 C16 1.386(13) .
C15 H15 0.9500 .
C16 C17 1.460(12) .
C17 H17 0.9500 .
C18 H18A 0.9800 .
C18 H18B 0.9800 .
C18 H18C 0.9800 .
