#------------------------------------------------------------------------------
#$Date: 2023-12-24 02:55:46 +0200 (Sun, 24 Dec 2023) $
#$Revision: 288539 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/31/25/4312528.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_4312528
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 Cu2 Fe Gd N14 O13'
_chemical_formula_weight         1111.01
_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                 129.767(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.510(9)
_cell_length_b                   10.130(3)
_cell_length_c                   19.055(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_volume                     4082(2)
_computing_cell_refinement       'SMART (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    'PLATON (Spek, 2002)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean '15\\times15 microns'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0384
_diffrn_reflns_av_sigmaI/netI    0.0449
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            11388
_diffrn_reflns_theta_full        26.39
_diffrn_reflns_theta_max         26.39
_diffrn_reflns_theta_min         2.23
_exptl_absorpt_coefficient_mu    3.056
_exptl_absorpt_correction_T_max  1.179
_exptl_absorpt_correction_T_min  0.875
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2000)'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.808
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2240
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.246
_refine_diff_density_min         -1.723
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         4184
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0392
_refine_ls_shift/su_max          0.036
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0500P)²+18.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0924
_refine_ls_wR_factor_ref         0.1003
_reflns_number_gt                3412
_reflns_number_total             4184
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0348502si20030718_093054_3.cif
_cod_data_source_block           3
_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 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'NONE' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4312528
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 0.92755(3) 0.2500 0.02491(11) Uani 1 2 d S . .
Fe1 Fe 0.2500 0.7500 0.5000 0.0225(2) Uani 1 2 d S . .
Cu1 Cu 0.11572(4) 0.77423(7) 0.60967(4) 0.0430(2) Uani 1 1 d . . .
N3 N 0.0825(2) 0.9378(5) 0.5394(3) 0.0402(11) Uani 1 1 d . . .
C3 C 0.1362(4) 0.4861(7) 0.6388(5) 0.072(2) Uani 1 1 d . . .
H3A H 0.1021 0.4616 0.6387 0.086 Uiso 1 1 calc R . .
H3B H 0.1700 0.4229 0.6773 0.086 Uiso 1 1 calc R . .
C13 C 0.2223(2) 0.5672(5) 0.4816(3) 0.0321(11) Uani 1 1 d . . .
C11 C 0.1639(2) 0.8122(5) 0.4066(3) 0.0282(10) Uani 1 1 d . . .
N4 N 0.0670(2) 0.6894(4) 0.4897(3) 0.0385(10) Uani 1 1 d . . .
O2 O 0.02692(18) 1.0040(4) 0.3897(2) 0.0393(9) Uani 1 1 d . . .
C9 C 0.0500(2) 0.9181(5) 0.4527(3) 0.0334(11) Uani 1 1 d . . .
N11 N 0.1132(2) 0.8492(5) 0.3524(3) 0.0383(10) Uani 1 1 d . . .
N13 N 0.2075(3) 0.4595(5) 0.4710(4) 0.0515(13) Uani 1 1 d . . .
C12 C 0.2604(2) 0.7243(5) 0.4087(3) 0.0325(11) Uani 1 1 d . . .
O1 O 0.00501(17) 0.7514(4) 0.3373(2) 0.0361(8) Uani 1 1 d . . .
N2 N 0.1617(3) 0.8604(5) 0.7308(3) 0.0638(17) Uani 1 1 d . . .
H2C H 0.1305 0.8598 0.7347 0.077 Uiso 1 1 calc R . .
C10 C 0.0396(2) 0.7736(5) 0.4240(3) 0.0307(11) Uani 1 1 d . . .
N12 N 0.2666(3) 0.7078(5) 0.3555(4) 0.0530(13) Uani 1 1 d . . .
C4 C 0.1886(4) 0.6320(7) 0.7749(4) 0.067(2) Uani 1 1 d . . .
H4A H 0.2270 0.5798 0.8123 0.081 Uiso 1 1 calc R . .
H4B H 0.1608 0.6011 0.7863 0.081 Uiso 1 1 calc R . .
C6 C 0.1743(4) 0.9960(7) 0.7408(4) 0.0618(19) Uani 1 1 d . . .
H6A H 0.2127 1.0083 0.7492 0.074 Uiso 1 1 calc R . .
H6B H 0.1836 1.0232 0.7971 0.074 Uiso 1 1 calc R . .
N1 N 0.1589(3) 0.6104(5) 0.6820(3) 0.0618(16) Uani 1 1 d . . .
H1C H 0.1937 0.6151 0.6863 0.074 Uiso 1 1 calc R . .
C1 C 0.0632(3) 0.5479(6) 0.4692(4) 0.0499(15) Uani 1 1 d . . .
H1A H 0.0650 0.5374 0.4204 0.060 Uiso 1 1 calc R . .
H1B H 0.0226 0.5144 0.4475 0.060 Uiso 1 1 calc R . .
C5 C 0.2044(3) 0.7695(7) 0.8025(4) 0.0575(18) Uani 1 1 d . . .
H5A H 0.2045 0.7848 0.8528 0.069 Uiso 1 1 calc R . .
H5B H 0.2468 0.7864 0.8243 0.069 Uiso 1 1 calc R . .
C2 C 0.1136(5) 0.4685(7) 0.5478(5) 0.085(3) Uani 1 1 d . . .
H2A H 0.1001 0.3772 0.5319 0.103 Uiso 1 1 calc R . .
H2B H 0.1501 0.4773 0.5512 0.103 Uiso 1 1 calc R . .
O1W O 0.06752(18) 1.1176(4) 0.2926(3) 0.0481(10) Uani 1 1 d . . .
O2W O 0.1684(2) 0.1872(5) 0.4641(3) 0.0644(13) Uani 1 1 d . . .
C8 C 0.0987(4) 1.0750(6) 0.5746(4) 0.0563(17) Uani 1 1 d . . .
H8A H 0.1275 1.1110 0.5666 0.068 Uiso 1 1 calc R . .
H8B H 0.0605 1.1279 0.5383 0.068 Uiso 1 1 calc R . .
O3W O 0.0236(3) 0.7423(6) 0.6249(5) 0.098(2) Uani 1 1 d . . .
O4W O -0.0778(3) 0.5415(7) 0.2390(4) 0.133(3) Uani 1 1 d . . .
C7 C 0.1275(5) 1.0870(7) 0.6702(5) 0.083(3) Uani 1 1 d . . .
H7A H 0.0930 1.0879 0.6719 0.100 Uiso 1 1 calc R . .
H7B H 0.1467 1.1739 0.6896 0.100 Uiso 1 1 calc R . .
O5W O 0.0000 1.3709(10) 0.2500 0.224(10) Uani 1 2 d S . .
H201 H 0.1791 0.2692 0.4701 0.050 Uiso 1 1 d . . .
H200 H 0.2036 0.1473 0.4884 0.050 Uiso 1 1 d . . .
H500 H 0.0308 1.4197 0.2646 0.050 Uiso 1 1 d . . .
H100 H 0.0997 1.1368 0.3496 0.050 Uiso 1 1 d . . .
H101 H 0.0488 1.1880 0.2667 0.050 Uiso 1 1 d . . .
H401 H -0.0529 0.6087 0.2679 0.050 Uiso 1 1 d . . .
H400 H -0.1031 0.5635 0.1817 0.050 Uiso 1 1 d . . .
H300 H 0.0084 0.6798 0.6381 0.050 Uiso 1 1 d . . .
H301 H 0.0081 0.8071 0.6358 0.050 Uiso 1 1 d . . .
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'
Fe Fe 0.3463 0.8444 '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 83.03(18) 2 . ?
O1 Gd1 O2 149.17(12) 2 . ?
O1 Gd1 O2 68.07(12) . . ?
O1 Gd1 O2 68.07(12) 2 2 ?
O1 Gd1 O2 149.17(12) . 2 ?
O2 Gd1 O2 142.19(18) . 2 ?
O1 Gd1 O1W 121.18(14) 2 . ?
O1 Gd1 O1W 132.11(12) . . ?
O2 Gd1 O1W 75.21(14) . . ?
O2 Gd1 O1W 74.99(13) 2 . ?
O1 Gd1 O1W 132.11(12) 2 2 ?
O1 Gd1 O1W 121.18(14) . 2 ?
O2 Gd1 O1W 74.99(13) . 2 ?
O2 Gd1 O1W 75.21(14) 2 2 ?
O1W Gd1 O1W 75.0(2) . 2 ?
O1 Gd1 N11 74.48(14) 2 2 ?
O1 Gd1 N11 78.24(14) . 2 ?
O2 Gd1 N11 108.28(14) . 2 ?
O2 Gd1 N11 83.71(14) 2 2 ?
O1W Gd1 N11 144.17(14) . 2 ?
O1W Gd1 N11 71.87(14) 2 2 ?
O1 Gd1 N11 78.24(14) 2 . ?
O1 Gd1 N11 74.48(14) . . ?
O2 Gd1 N11 83.71(14) . . ?
O2 Gd1 N11 108.28(14) 2 . ?
O1W Gd1 N11 71.87(14) . . ?
O1W Gd1 N11 144.17(14) 2 . ?
N11 Gd1 N11 143.3(2) 2 . ?
C11 Fe1 C11 180.000(1) 7_566 . ?
C11 Fe1 C13 87.9(2) 7_566 . ?
C11 Fe1 C13 92.1(2) . . ?
C11 Fe1 C13 92.1(2) 7_566 7_566 ?
C11 Fe1 C13 87.9(2) . 7_566 ?
C13 Fe1 C13 180.000(1) . 7_566 ?
C11 Fe1 C12 89.2(2) 7_566 . ?
C11 Fe1 C12 90.8(2) . . ?
C13 Fe1 C12 88.6(2) . . ?
C13 Fe1 C12 91.4(2) 7_566 . ?
C11 Fe1 C12 90.8(2) 7_566 7_566 ?
C11 Fe1 C12 89.2(2) . 7_566 ?
C13 Fe1 C12 91.4(2) . 7_566 ?
C13 Fe1 C12 88.6(2) 7_566 7_566 ?
C12 Fe1 C12 180.00(7) . 7_566 ?
N3 Cu1 N4 84.33(18) . . ?
N3 Cu1 N2 95.4(2) . . ?
N4 Cu1 N2 177.5(3) . . ?
N3 Cu1 N1 172.8(3) . . ?
N4 Cu1 N1 95.8(2) . . ?
N2 Cu1 N1 84.7(2) . . ?
C9 N3 C8 118.9(5) . . ?
C9 N3 Cu1 112.5(4) . . ?
C8 N3 Cu1 127.7(4) . . ?
N1 C3 C2 120.3(7) . . ?
N1 C3 H3A 107.2 . . ?
C2 C3 H3A 107.2 . . ?
N1 C3 H3B 107.2 . . ?
C2 C3 H3B 107.2 . . ?
H3A C3 H3B 106.9 . . ?
N13 C13 Fe1 178.2(5) . . ?
N11 C11 Fe1 179.2(5) . . ?
C10 N4 C1 119.3(5) . . ?
C10 N4 Cu1 112.5(4) . . ?
C1 N4 Cu1 128.0(3) . . ?
C9 O2 Gd1 116.1(3) . . ?
O2 C9 N3 128.1(5) . . ?
O2 C9 C10 116.9(4) . . ?
N3 C9 C10 115.1(4) . . ?
C11 N11 Gd1 172.1(4) . . ?
N12 C12 Fe1 179.2(5) . . ?
C10 O1 Gd1 115.3(3) . . ?
C6 N2 C5 121.5(6) . . ?
C6 N2 Cu1 120.5(4) . . ?
C5 N2 Cu1 110.5(4) . . ?
C6 N2 H2C 99.2 . . ?
C5 N2 H2C 99.2 . . ?
Cu1 N2 H2C 99.2 . . ?
N4 C10 O1 128.5(5) . . ?
N4 C10 C9 115.3(4) . . ?
O1 C10 C9 116.2(4) . . ?
N1 C4 C5 113.6(6) . . ?
N1 C4 H4A 108.8 . . ?
C5 C4 H4A 108.8 . . ?
N1 C4 H4B 108.8 . . ?
C5 C4 H4B 108.8 . . ?
H4A C4 H4B 107.7 . . ?
N2 C6 C7 120.2(6) . . ?
N2 C6 H6A 107.3 . . ?
C7 C6 H6A 107.3 . . ?
N2 C6 H6B 107.3 . . ?
C7 C6 H6B 107.3 . . ?
H6A C6 H6B 106.9 . . ?
C4 N1 C3 123.6(6) . . ?
C4 N1 Cu1 110.4(4) . . ?
C3 N1 Cu1 119.6(4) . . ?
C4 N1 H1C 98.4 . . ?
C3 N1 H1C 98.4 . . ?
Cu1 N1 H1C 98.4 . . ?
N4 C1 C2 113.7(5) . . ?
N4 C1 H1A 108.8 . . ?
C2 C1 H1A 108.8 . . ?
N4 C1 H1B 108.8 . . ?
C2 C1 H1B 108.8 . . ?
H1A C1 H1B 107.7 . . ?
N2 C5 C4 113.6(6) . . ?
N2 C5 H5A 108.9 . . ?
C4 C5 H5A 108.9 . . ?
N2 C5 H5B 108.9 . . ?
C4 C5 H5B 108.9 . . ?
H5A C5 H5B 107.7 . . ?
C3 C2 C1 124.2(7) . . ?
C3 C2 H2A 106.3 . . ?
C1 C2 H2A 106.3 . . ?
C3 C2 H2B 106.3 . . ?
C1 C2 H2B 106.3 . . ?
H2A C2 H2B 106.4 . . ?
Gd1 O1W H100 122.7 . . ?
Gd1 O1W H101 115.5 . . ?
H100 O1W H101 107.2 . . ?
H201 O2W H200 102.1 . . ?
C7 C8 N3 114.2(5) . . ?
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 . . ?
H300 O3W H301 94.7 . . ?
H401 O4W H400 105.6 . . ?
C8 C7 C6 124.0(7) . . ?
C8 C7 H7A 106.3 . . ?
C6 C7 H7A 106.3 . . ?
C8 C7 H7B 106.3 . . ?
C6 C7 H7B 106.3 . . ?
H7A C7 H7B 106.4 . . ?
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 2.383(4) 2 ?
Gd1 O1 2.383(4) . ?
Gd1 O2 2.391(4) . ?
Gd1 O2 2.391(4) 2 ?
Gd1 O1W 2.426(4) . ?
Gd1 O1W 2.426(4) 2 ?
Gd1 N11 2.522(4) 2 ?
Gd1 N11 2.522(4) . ?
Fe1 C11 1.944(5) 7_566 ?
Fe1 C11 1.944(5) . ?
Fe1 C13 1.947(5) . ?
Fe1 C13 1.947(5) 7_566 ?
Fe1 C12 1.953(5) . ?
Fe1 C12 1.953(5) 7_566 ?
Cu1 N3 1.951(5) . ?
Cu1 N4 1.959(4) . ?
Cu1 N2 1.989(5) . ?
Cu1 N1 1.992(5) . ?
N3 C9 1.296(6) . ?
N3 C8 1.483(7) . ?
C3 N1 1.412(9) . ?
C3 C2 1.430(10) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C13 N13 1.136(7) . ?
C11 N11 1.145(6) . ?
N4 C10 1.287(6) . ?
N4 C1 1.471(7) . ?
O2 C9 1.275(6) . ?
C9 C10 1.524(7) . ?
C12 N12 1.142(7) . ?
O1 C10 1.293(6) . ?
N2 C6 1.399(8) . ?
N2 C5 1.428(8) . ?
N2 H2C 0.9100 . ?
C4 N1 1.413(8) . ?
C4 C5 1.454(10) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C6 C7 1.449(10) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
N1 H1C 0.9100 . ?
C1 C2 1.469(9) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
O1W H100 0.8782 . ?
O1W H101 0.8323 . ?
O2W H201 0.8635 . ?
O2W H200 0.8617 . ?
C8 C7 1.453(9) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
O3W H300 0.8792 . ?
O3W H301 0.8759 . ?
O4W H401 0.8668 . ?
O4W H400 0.8689 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
O5W H500 0.8583 . ?
