#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:58:35 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179164 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/25/4312529.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_4312529
loop_
_publ_author_name
'Hui-Zhong Kou'
'Bei Chuan Zhou'
'Ru-Ji Wang'
_publ_contact_author_address
;
Department of Chemistry
Tsinghua University
Beijing 100084
People's Republic of China
;
_publ_contact_author_email       kouhz@mail.tsinghua.edu.cn
_publ_contact_author_fax         86-10-62788765
_publ_contact_author_name        'Hui-Zhong Kou'
_publ_contact_author_phone       86(10)62795529
_publ_section_title
;
 Heterotrimetallic 4f-3d Coordination Polymers: Synthesis, Crystal
 Structure, and Magnetic Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7658
_journal_page_last               7665
_journal_paper_doi               10.1021/ic0348502
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C26 H54 Cr Cu2 Gd N14 O13'
_chemical_formula_weight         1107.16
_chemical_name_systematic
; 
 ? 
;
_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                 129.622(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   28.006(8)
_cell_length_b                   10.1441(18)
_cell_length_c                   19.041(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_volume                     4166.7(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Siemens Bruker P4'
_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  0.0233
_diffrn_reflns_av_sigmaI/netI    0.0404
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            4398
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.89
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.906
_exptl_absorpt_correction_T_max  0.943
_exptl_absorpt_correction_T_min  0.802
_exptl_absorpt_correction_type   emperical
_exptl_crystal_colour            Violet
_exptl_crystal_density_diffrn    1.765
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2232
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.628
_refine_diff_density_min         -1.370
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         3669
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0414
_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)+(0.0600P)²+10.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1049
_refine_ls_wR_factor_ref         0.1093
_reflns_number_gt                3231
_reflns_number_total             3669
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0348502si20030718_093054_4.cif
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        4166.8(15)
_cod_database_code               4312529
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd1 Gd 0.0000 0.93239(3) 0.2500 0.03426(13) Uani 1 2 d S . .
Cr1 Cr 0.2500 0.7500 0.5000 0.0324(2) Uani 1 2 d S . .
Cu1 Cu 0.11478(4) 0.77518(7) 0.60913(4) 0.0536(2) Uani 1 1 d . . .
N3 N 0.0822(2) 0.9384(5) 0.5397(3) 0.0531(12) Uani 1 1 d . . .
C3 C 0.1348(4) 0.4878(7) 0.6373(5) 0.085(2) Uani 1 1 d . . .
H3A H 0.1020 0.4627 0.6387 0.102 Uiso 1 1 calc R . .
H3B H 0.1682 0.4249 0.6751 0.102 Uiso 1 1 calc R . .
C13 C 0.2194(2) 0.5564(5) 0.4799(3) 0.0434(12) Uani 1 1 d . . .
C11 C 0.1602(2) 0.8171(5) 0.4022(3) 0.0394(11) Uani 1 1 d . . .
N4 N 0.0672(2) 0.6915(5) 0.4891(3) 0.0499(11) Uani 1 1 d . . .
O2 O 0.02675(18) 1.0060(4) 0.3902(2) 0.0502(9) Uani 1 1 d . . .
C9 C 0.0502(2) 0.9199(5) 0.4532(3) 0.0428(11) Uani 1 1 d . . .
N11 N 0.1102(2) 0.8553(5) 0.3497(3) 0.0484(10) Uani 1 1 d . . .
N13 N 0.2050(3) 0.4500(5) 0.4694(4) 0.0650(14) Uani 1 1 d . . .
C12 C 0.2593(2) 0.7217(5) 0.4015(3) 0.0427(11) Uani 1 1 d . . .
O1 O 0.00597(16) 0.7544(4) 0.3372(2) 0.0455(8) Uani 1 1 d . . .
N2 N 0.1608(3) 0.8609(6) 0.7304(3) 0.0766(17) Uani 1 1 d . . .
H2C H 0.1301 0.8599 0.7344 0.092 Uiso 1 1 calc R . .
C10 C 0.0397(2) 0.7768(5) 0.4233(3) 0.0440(12) Uani 1 1 d . . .
N12 N 0.2655(3) 0.7029(6) 0.3486(4) 0.0674(14) Uani 1 1 d . . .
C4 C 0.1873(4) 0.6328(7) 0.7736(4) 0.078(2) Uani 1 1 d . . .
H4A H 0.2254 0.5821 0.8100 0.094 Uiso 1 1 calc R . .
H4B H 0.1610 0.5996 0.7863 0.094 Uiso 1 1 calc R . .
C6 C 0.1724(4) 0.9955(7) 0.7409(4) 0.074(2) Uani 1 1 d . . .
H6A H 0.2108 1.0088 0.7514 0.088 Uiso 1 1 calc R . .
H6B H 0.1801 1.0214 0.7964 0.088 Uiso 1 1 calc R . .
N1 N 0.1572(3) 0.6118(6) 0.6806(4) 0.0726(16) Uani 1 1 d . . .
H1C H 0.1911 0.6167 0.6839 0.087 Uiso 1 1 calc R . .
C1 C 0.0637(3) 0.5512(6) 0.4685(4) 0.0617(16) Uani 1 1 d . . .
H1A H 0.0667 0.5415 0.4208 0.074 Uiso 1 1 calc R . .
H1B H 0.0234 0.5183 0.4449 0.074 Uiso 1 1 calc R . .
C5 C 0.2018(3) 0.7691(7) 0.8016(4) 0.0665(17) Uani 1 1 d . . .
H5A H 0.2007 0.7830 0.8510 0.080 Uiso 1 1 calc R . .
H5B H 0.2437 0.7867 0.8251 0.080 Uiso 1 1 calc R . .
C2 C 0.1116(5) 0.4697(8) 0.5464(5) 0.101(3) Uani 1 1 d . . .
H2A H 0.0966 0.3797 0.5302 0.122 Uiso 1 1 calc R . .
H2B H 0.1473 0.4737 0.5490 0.122 Uiso 1 1 calc R . .
O1W O 0.06624(18) 1.1223(4) 0.2934(3) 0.0580(10) Uani 1 1 d . . .
O2W O 0.1681(2) 0.1815(5) 0.4651(3) 0.0751(13) Uani 1 1 d . . .
C8 C 0.0982(4) 1.0756(6) 0.5747(5) 0.072(2) Uani 1 1 d . . .
H8A H 0.1256 1.1121 0.5651 0.086 Uiso 1 1 calc R . .
H8B H 0.0606 1.1280 0.5397 0.086 Uiso 1 1 calc R . .
O3W O 0.0239(3) 0.7427(6) 0.6246(5) 0.1047(19) Uani 1 1 d . . .
O4W O -0.0761(4) 0.5468(8) 0.2413(5) 0.142(3) Uani 1 1 d . . .
C7 C 0.1279(5) 1.0870(7) 0.6711(5) 0.101(3) Uani 1 1 d . . .
H7A H 0.1480 1.1725 0.6904 0.121 Uiso 1 1 calc R . .
H7B H 0.0946 1.0917 0.6739 0.121 Uiso 1 1 calc R . .
O5W O 0.0000 1.3737(11) 0.2500 0.242(11) Uani 1 2 d S . .
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'
Cr Cr 0.3209 0.6236 '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'
N N 0.0061 0.0033 '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
O1 Gd1 O1 81.64(17) 2 . ?
O1 Gd1 O2 148.02(12) 2 . ?
O1 Gd1 O2 68.00(13) . . ?
O1 Gd1 O2 68.00(13) 2 2 ?
O1 Gd1 O2 148.02(12) . 2 ?
O2 Gd1 O2 143.52(18) . 2 ?
O1 Gd1 O1W 122.47(15) 2 . ?
O1 Gd1 O1W 131.71(12) . . ?
O2 Gd1 O1W 75.19(14) . . ?
O2 Gd1 O1W 76.02(13) 2 . ?
O1 Gd1 O1W 131.71(12) 2 2 ?
O1 Gd1 O1W 122.47(15) . 2 ?
O2 Gd1 O1W 76.02(13) . 2 ?
O2 Gd1 O1W 75.19(14) 2 2 ?
O1W Gd1 O1W 74.8(2) . 2 ?
O1 Gd1 N11 74.37(14) 2 2 ?
O1 Gd1 N11 78.27(14) . 2 ?
O2 Gd1 N11 107.56(15) . 2 ?
O2 Gd1 N11 83.91(14) 2 2 ?
O1W Gd1 N11 144.27(14) . 2 ?
O1W Gd1 N11 71.60(15) 2 2 ?
O1 Gd1 N11 78.27(14) 2 . ?
O1 Gd1 N11 74.37(14) . . ?
O2 Gd1 N11 83.91(14) . . ?
O2 Gd1 N11 107.56(15) 2 . ?
O1W Gd1 N11 71.60(15) . . ?
O1W Gd1 N11 144.27(15) 2 . ?
N11 Gd1 N11 143.6(2) 2 . ?
C11 Cr1 C11 180.000(1) 7_566 . ?
C11 Cr1 C12 90.73(19) 7_566 7_566 ?
C11 Cr1 C12 89.27(19) . 7_566 ?
C11 Cr1 C12 89.27(19) 7_566 . ?
C11 Cr1 C12 90.73(19) . . ?
C12 Cr1 C12 180.000(1) 7_566 . ?
C11 Cr1 C13 88.7(2) 7_566 . ?
C11 Cr1 C13 91.3(2) . . ?
C12 Cr1 C13 91.3(2) 7_566 . ?
C12 Cr1 C13 88.7(2) . . ?
C11 Cr1 C13 91.3(2) 7_566 7_566 ?
C11 Cr1 C13 88.7(2) . 7_566 ?
C12 Cr1 C13 88.7(2) 7_566 7_566 ?
C12 Cr1 C13 91.3(2) . 7_566 ?
C13 Cr1 C13 180.000(1) . 7_566 ?
N3 Cu1 N4 84.31(19) . . ?
N3 Cu1 N1 172.7(3) . . ?
N4 Cu1 N1 95.9(2) . . ?
N3 Cu1 N2 95.3(2) . . ?
N4 Cu1 N2 178.3(3) . . ?
N1 Cu1 N2 84.7(2) . . ?
C9 N3 C8 118.4(5) . . ?
C9 N3 Cu1 112.7(4) . . ?
C8 N3 Cu1 128.1(4) . . ?
N1 C3 C2 120.9(7) . . ?
N1 C3 H3A 107.1 . . ?
C2 C3 H3A 107.1 . . ?
N1 C3 H3B 107.1 . . ?
C2 C3 H3B 107.1 . . ?
H3A C3 H3B 106.8 . . ?
N13 C13 Cr1 177.0(5) . . ?
N11 C11 Cr1 178.0(4) . . ?
C10 N4 C1 119.6(5) . . ?
C10 N4 Cu1 112.4(4) . . ?
C1 N4 Cu1 127.9(4) . . ?
C9 O2 Gd1 116.3(3) . . ?
O2 C9 N3 128.4(5) . . ?
O2 C9 C10 116.2(4) . . ?
N3 C9 C10 115.4(4) . . ?
C11 N11 Gd1 173.0(4) . . ?
N12 C12 Cr1 178.0(5) . . ?
C10 O1 Gd1 115.0(3) . . ?
C6 N2 C5 122.2(5) . . ?
C6 N2 Cu1 121.0(4) . . ?
C5 N2 Cu1 110.5(4) . . ?
C6 N2 H2C 98.3 . . ?
C5 N2 H2C 98.3 . . ?
Cu1 N2 H2C 98.3 . . ?
O1 C10 N4 127.9(5) . . ?
O1 C10 C9 117.2(4) . . ?
N4 C10 C9 114.9(4) . . ?
N1 C4 C5 114.2(6) . . ?
N1 C4 H4A 108.7 . . ?
C5 C4 H4A 108.7 . . ?
N1 C4 H4B 108.7 . . ?
C5 C4 H4B 108.7 . . ?
H4A C4 H4B 107.6 . . ?
N2 C6 C7 121.2(6) . . ?
N2 C6 H6A 107.0 . . ?
C7 C6 H6A 107.0 . . ?
N2 C6 H6B 107.0 . . ?
C7 C6 H6B 107.0 . . ?
H6A C6 H6B 106.8 . . ?
C4 N1 C3 123.7(6) . . ?
C4 N1 Cu1 110.6(5) . . ?
C3 N1 Cu1 119.6(4) . . ?
C4 N1 H1C 98.3 . . ?
C3 N1 H1C 98.3 . . ?
Cu1 N1 H1C 98.3 . . ?
N4 C1 C2 114.6(5) . . ?
N4 C1 H1A 108.6 . . ?
C2 C1 H1A 108.6 . . ?
N4 C1 H1B 108.6 . . ?
C2 C1 H1B 108.6 . . ?
H1A C1 H1B 107.6 . . ?
N2 C5 C4 114.1(5) . . ?
N2 C5 H5A 108.7 . . ?
C4 C5 H5A 108.7 . . ?
N2 C5 H5B 108.7 . . ?
C4 C5 H5B 108.7 . . ?
H5A C5 H5B 107.6 . . ?
C3 C2 C1 124.9(8) . . ?
C3 C2 H2A 106.1 . . ?
C1 C2 H2A 106.1 . . ?
C3 C2 H2B 106.1 . . ?
C1 C2 H2B 106.1 . . ?
H2A C2 H2B 106.3 . . ?
C7 C8 N3 114.0(6) . . ?
C7 C8 H8A 108.7 . . ?
N3 C8 H8A 108.7 . . ?
C7 C8 H8B 108.7 . . ?
N3 C8 H8B 108.7 . . ?
H8A C8 H8B 107.6 . . ?
C6 C7 C8 125.1(8) . . ?
C6 C7 H7A 106.0 . . ?
C8 C7 H7A 106.0 . . ?
C6 C7 H7B 106.0 . . ?
C8 C7 H7B 106.0 . . ?
H7A C7 H7B 106.3 . . ?
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
Gd1 O1 2.386(4) 2 ?
Gd1 O1 2.386(4) . ?
Gd1 O2 2.387(3) . ?
Gd1 O2 2.387(3) 2 ?
Gd1 O1W 2.425(4) . ?
Gd1 O1W 2.425(4) 2 ?
Gd1 N11 2.504(4) 2 ?
Gd1 N11 2.504(4) . ?
Cr1 C11 2.069(5) 7_566 ?
Cr1 C11 2.069(5) . ?
Cr1 C12 2.072(5) 7_566 ?
Cr1 C12 2.072(5) . ?
Cr1 C13 2.078(6) . ?
Cr1 C13 2.078(6) 7_566 ?
Cu1 N3 1.945(5) . ?
Cu1 N4 1.959(4) . ?
Cu1 N1 1.987(5) . ?
Cu1 N2 1.989(5) . ?
N3 C9 1.291(7) . ?
N3 C8 1.483(8) . ?
C3 N1 1.413(9) . ?
C3 C2 1.420(10) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C13 N13 1.124(7) . ?
C11 N11 1.151(6) . ?
N4 C10 1.297(7) . ?
N4 C1 1.462(7) . ?
O2 C9 1.277(6) . ?
C9 C10 1.519(7) . ?
C12 N12 1.141(7) . ?
O1 C10 1.286(6) . ?
N2 C6 1.388(9) . ?
N2 C5 1.428(8) . ?
N2 H2C 0.9100 . ?
C4 N1 1.410(8) . ?
C4 C5 1.444(10) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C6 C7 1.438(10) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
N1 H1C 0.9100 . ?
C1 C2 1.466(10) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C8 C7 1.457(10) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
