#------------------------------------------------------------------------------
#$Date: 2023-12-24 02:55:46 +0200 (Sun, 24 Dec 2023) $
#$Revision: 288539 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/31/25/4312526.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_4312526
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 Co Cu2 Gd N14 O13'
_chemical_formula_weight         1114.09
_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                 129.810(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.413(8)
_cell_length_b                   10.130(3)
_cell_length_c                   19.067(5)
_cell_measurement_temperature    293(2)
_cell_volume                     4067(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 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0419
_diffrn_reflns_av_sigmaI/netI    0.0579
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7387
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.23
_exptl_absorpt_coefficient_mu    3.118
_exptl_absorpt_correction_T_max  1.148
_exptl_absorpt_correction_T_min  0.996
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2000)'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.819
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2244
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.941
_refine_diff_density_min         -0.787
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         3550
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0405
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0388P)²+14.0099P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0822
_refine_ls_wR_factor_ref         0.0886
_reflns_number_gt                2788
_reflns_number_total             3550
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0348502si20030718_093054_1.cif
_cod_data_source_block           1
_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_database_code               4312526
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 0.92398(4) 0.2500 0.02248(13) Uani 1 2 d S . .
Co1 Co 0.2500 0.7500 0.5000 0.0206(2) Uani 1 2 d S . .
Cu1 Cu 0.11588(4) 0.77239(8) 0.60944(5) 0.0437(2) Uani 1 1 d . . .
N3 N 0.0823(2) 0.9357(5) 0.5387(3) 0.0407(13) Uani 1 1 d . . .
C3 C 0.1362(4) 0.4848(8) 0.6384(5) 0.071(3) Uani 1 1 d . . .
H3A H 0.1704 0.4219 0.6768 0.085 Uiso 1 1 calc R . .
H3B H 0.1021 0.4594 0.6384 0.085 Uiso 1 1 calc R . .
C13 C 0.2230(2) 0.5711(7) 0.4817(3) 0.0276(12) Uani 1 1 d . . .
C11 C 0.1646(3) 0.8078(6) 0.4080(4) 0.0257(13) Uani 1 1 d . . .
N4 N 0.0674(2) 0.6862(5) 0.4901(3) 0.0375(13) Uani 1 1 d . . .
O2 O 0.0269(2) 1.0013(4) 0.3897(2) 0.0369(10) Uani 1 1 d . . .
C9 C 0.0499(3) 0.9151(6) 0.4522(4) 0.0348(14) Uani 1 1 d . . .
N11 N 0.1141(2) 0.8456(5) 0.3542(3) 0.0357(12) Uani 1 1 d . . .
N13 N 0.2083(3) 0.4627(6) 0.4713(4) 0.0478(15) Uani 1 1 d . . .
C12 C 0.2604(3) 0.7265(6) 0.4109(4) 0.0268(13) Uani 1 1 d . . .
O1 O 0.00472(18) 0.7483(4) 0.3372(2) 0.0342(10) Uani 1 1 d . . .
N2 N 0.1630(3) 0.8588(6) 0.7303(3) 0.0639(19) Uani 1 1 d . . .
H2C H 0.1314 0.8574 0.7338 0.077 Uiso 1 1 calc R . .
C10 C 0.0398(3) 0.7710(6) 0.4238(4) 0.0325(14) Uani 1 1 d . . .
N12 N 0.2665(3) 0.7112(6) 0.3576(4) 0.0478(15) Uani 1 1 d . . .
C4 C 0.1894(4) 0.6305(8) 0.7743(4) 0.065(2) Uani 1 1 d . . .
H4A H 0.2284 0.5794 0.8110 0.078 Uiso 1 1 calc R . .
H4B H 0.1625 0.5981 0.7870 0.078 Uiso 1 1 calc R . .
C6 C 0.1737(4) 0.9950(7) 0.7400(5) 0.059(2) Uani 1 1 d . . .
H6A H 0.2136 1.0094 0.7524 0.070 Uiso 1 1 calc R . .
H6B H 0.1804 1.0212 0.7945 0.070 Uiso 1 1 calc R . .
N1 N 0.1587(3) 0.6088(6) 0.6820(4) 0.0614(18) Uani 1 1 d . . .
H1C H 0.1935 0.6135 0.6859 0.074 Uiso 1 1 calc R . .
C1 C 0.0635(3) 0.5461(6) 0.4693(4) 0.0498(19) Uani 1 1 d . . .
H1A H 0.0662 0.5359 0.4213 0.060 Uiso 1 1 calc R . .
H1B H 0.0225 0.5125 0.4464 0.060 Uiso 1 1 calc R . .
C5 C 0.2048(4) 0.7681(8) 0.8022(4) 0.055(2) Uani 1 1 d . . .
H5A H 0.2034 0.7833 0.8512 0.066 Uiso 1 1 calc R . .
H5B H 0.2478 0.7852 0.8260 0.066 Uiso 1 1 calc R . .
C2 C 0.1138(5) 0.4670(9) 0.5486(5) 0.091(3) Uani 1 1 d . . .
H2A H 0.0999 0.3758 0.5329 0.109 Uiso 1 1 calc R . .
H2B H 0.1506 0.4745 0.5523 0.109 Uiso 1 1 calc R . .
O1W O 0.06769(19) 1.1136(4) 0.2926(3) 0.0434(11) Uani 1 1 d . . .
O2W O 0.1685(2) 0.1901(5) 0.4627(3) 0.0614(14) Uani 1 1 d . . .
C8 C 0.0985(4) 1.0721(7) 0.5740(5) 0.0546(19) Uani 1 1 d . . .
H8A H 0.1264 1.1089 0.5642 0.066 Uiso 1 1 calc R . .
H8B H 0.0599 1.1244 0.5387 0.066 Uiso 1 1 calc R . .
O3W O 0.0234(3) 0.7449(6) 0.6251(4) 0.0894(19) Uani 1 1 d . . .
O4W O -0.0785(3) 0.5396(7) 0.2382(4) 0.128(3) Uani 1 1 d . . .
C7 C 0.1290(5) 1.0849(9) 0.6698(5) 0.097(4) Uani 1 1 d . . .
H7A H 0.1499 1.1703 0.6886 0.117 Uiso 1 1 calc R . .
H7B H 0.0950 1.0916 0.6724 0.117 Uiso 1 1 calc R . .
O5W O 0.0000 1.3660(12) 0.2500 0.215(9) 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'
Co Co 0.3494 0.9721 '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 83.27(19) 2 . ?
O1 Gd1 O2 149.43(14) 2 . ?
O1 Gd1 O2 68.14(13) . . ?
O1 Gd1 O2 68.14(13) 2 2 ?
O1 Gd1 O2 149.43(14) . 2 ?
O2 Gd1 O2 141.8(2) . 2 ?
O1 Gd1 O1W 120.97(15) 2 . ?
O1 Gd1 O1W 132.15(13) . . ?
O2 Gd1 O1W 75.14(15) . . ?
O2 Gd1 O1W 74.80(14) 2 . ?
O1 Gd1 O1W 132.15(13) 2 2 ?
O1 Gd1 O1W 120.98(15) . 2 ?
O2 Gd1 O1W 74.80(14) . 2 ?
O2 Gd1 O1W 75.14(15) 2 2 ?
O1W Gd1 O1W 75.0(2) . 2 ?
O1 Gd1 N11 74.33(15) 2 2 ?
O1 Gd1 N11 78.53(15) . 2 ?
O2 Gd1 N11 108.73(15) . 2 ?
O2 Gd1 N11 83.34(15) 2 2 ?
O1W Gd1 N11 143.99(15) . 2 ?
O1W Gd1 N11 71.87(15) 2 2 ?
O1 Gd1 N11 78.53(15) 2 . ?
O1 Gd1 N11 74.33(15) . . ?
O2 Gd1 N11 83.34(15) . . ?
O2 Gd1 N11 108.73(15) 2 . ?
O1W Gd1 N11 71.87(15) . . ?
O1W Gd1 N11 143.99(15) 2 . ?
N11 Gd1 N11 143.4(2) 2 . ?
C13 Co1 C13 180.000(1) . 7_566 ?
C13 Co1 C12 88.9(2) . . ?
C13 Co1 C12 91.1(2) 7_566 . ?
C13 Co1 C12 91.1(2) . 7_566 ?
C13 Co1 C12 88.9(2) 7_566 7_566 ?
C12 Co1 C12 180.00(7) . 7_566 ?
C13 Co1 C11 91.1(2) . . ?
C13 Co1 C11 88.9(2) 7_566 . ?
C12 Co1 C11 90.8(2) . . ?
C12 Co1 C11 89.2(2) 7_566 . ?
C13 Co1 C11 88.9(2) . 7_566 ?
C13 Co1 C11 91.1(2) 7_566 7_566 ?
C12 Co1 C11 89.2(2) . 7_566 ?
C12 Co1 C11 90.8(2) 7_566 7_566 ?
C11 Co1 C11 180.000(2) . 7_566 ?
N3 Cu1 N4 84.6(2) . . ?
N3 Cu1 N2 95.5(2) . . ?
N4 Cu1 N2 178.4(3) . . ?
N3 Cu1 N1 173.3(3) . . ?
N4 Cu1 N1 95.5(2) . . ?
N2 Cu1 N1 84.5(2) . . ?
C9 N3 C8 119.4(5) . . ?
C9 N3 Cu1 112.3(4) . . ?
C8 N3 Cu1 127.4(4) . . ?
C2 C3 N1 121.0(7) . . ?
C2 C3 H3A 107.1 . . ?
N1 C3 H3A 107.1 . . ?
C2 C3 H3B 107.1 . . ?
N1 C3 H3B 107.1 . . ?
H3A C3 H3B 106.8 . . ?
N13 C13 Co1 178.1(5) . . ?
N11 C11 Co1 178.2(5) . . ?
C10 N4 C1 118.9(5) . . ?
C10 N4 Cu1 112.0(4) . . ?
C1 N4 Cu1 128.8(4) . . ?
C9 O2 Gd1 115.6(4) . . ?
O2 C9 N3 127.4(6) . . ?
O2 C9 C10 117.3(5) . . ?
N3 C9 C10 115.3(5) . . ?
C11 N11 Gd1 172.5(5) . . ?
N12 C12 Co1 179.4(6) . . ?
C10 O1 Gd1 115.0(4) . . ?
C6 N2 C5 122.6(6) . . ?
C6 N2 Cu1 121.0(5) . . ?
C5 N2 Cu1 111.0(5) . . ?
C6 N2 H2C 97.8 . . ?
C5 N2 H2C 97.8 . . ?
Cu1 N2 H2C 97.8 . . ?
O1 C10 N4 128.3(6) . . ?
O1 C10 C9 116.3(5) . . ?
N4 C10 C9 115.4(5) . . ?
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 121.8(7) . . ?
N2 C6 H6A 106.9 . . ?
C7 C6 H6A 106.9 . . ?
N2 C6 H6B 106.9 . . ?
C7 C6 H6B 106.9 . . ?
H6A C6 H6B 106.7 . . ?
C4 N1 C3 124.4(6) . . ?
C4 N1 Cu1 110.9(5) . . ?
C3 N1 Cu1 119.4(4) . . ?
C4 N1 H1C 97.7 . . ?
C3 N1 H1C 97.7 . . ?
Cu1 N1 H1C 97.7 . . ?
N4 C1 C2 113.2(6) . . ?
N4 C1 H1A 108.9 . . ?
C2 C1 H1A 108.9 . . ?
N4 C1 H1B 108.9 . . ?
C2 C1 H1B 108.9 . . ?
H1A C1 H1B 107.8 . . ?
N2 C5 C4 113.6(6) . . ?
N2 C5 H5A 108.8 . . ?
C4 C5 H5A 108.8 . . ?
N2 C5 H5B 108.8 . . ?
C4 C5 H5B 108.8 . . ?
H5A C5 H5B 107.7 . . ?
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 . . ?
Gd1 O1W H100 124.5 . . ?
Gd1 O1W H101 116.6 . . ?
H100 O1W H101 103.2 . . ?
H201 O2W H200 104.0 . . ?
C7 C8 N3 114.9(6) . . ?
C7 C8 H8A 108.5 . . ?
N3 C8 H8A 108.5 . . ?
C7 C8 H8B 108.6 . . ?
N3 C8 H8B 108.5 . . ?
H8A C8 H8B 107.5 . . ?
H300 O3W H301 95.3 . . ?
H401 O4W H400 103.9 . . ?
C6 C7 C8 125.7(8) . . ?
C6 C7 H7A 105.9 . . ?
C8 C7 H7A 105.9 . . ?
C6 C7 H7B 105.9 . . ?
C8 C7 H7B 105.9 . . ?
H7A C7 H7B 106.2 . . ?
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 2.381(4) 2 ?
Gd1 O1 2.381(4) . ?
Gd1 O2 2.396(4) . ?
Gd1 O2 2.396(4) 2 ?
Gd1 O1W 2.421(4) . ?
Gd1 O1W 2.421(4) 2 ?
Gd1 N11 2.531(5) 2 ?
Gd1 N11 2.531(5) . ?
Co1 C13 1.903(7) . ?
Co1 C13 1.903(7) 7_566 ?
Co1 C12 1.908(6) . ?
Co1 C12 1.908(6) 7_566 ?
Co1 C11 1.908(5) . ?
Co1 C11 1.908(5) 7_566 ?
Cu1 N3 1.952(5) . ?
Cu1 N4 1.958(5) . ?
Cu1 N2 1.983(6) . ?
Cu1 N1 1.989(6) . ?
N3 C9 1.296(7) . ?
N3 C8 1.475(8) . ?
C3 C2 1.411(10) . ?
C3 N1 1.411(9) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C13 N13 1.142(7) . ?
C11 N11 1.139(7) . ?
N4 C10 1.297(7) . ?
N4 C1 1.459(8) . ?
O2 C9 1.271(7) . ?
C9 C10 1.520(9) . ?
C12 N12 1.142(7) . ?
O1 C10 1.294(7) . ?
N2 C6 1.398(9) . ?
N2 C5 1.423(8) . ?
N2 H2C 0.9100 . ?
C4 N1 1.400(8) . ?
C4 C5 1.455(10) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C6 C7 1.422(10) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
N1 H1C 0.9100 . ?
C1 C2 1.470(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 . ?
O1W H100 0.8859 . ?
O1W H101 0.8681 . ?
O2W H201 0.8332 . ?
O2W H200 0.8672 . ?
C8 C7 1.448(9) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
O3W H300 0.8937 . ?
O3W H301 0.8518 . ?
O4W H401 0.8907 . ?
O4W H400 0.8628 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
O5W H500 0.8849 . ?
