#------------------------------------------------------------------------------
#$Date: 2023-12-24 02:55:46 +0200 (Sun, 24 Dec 2023) $
#$Revision: 288539 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/31/25/4312527.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_4312527
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 La N14 O13'
_chemical_formula_weight         1092.67
_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                 129.075(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.746(10)
_cell_length_b                   10.096(4)
_cell_length_c                   19.083(7)
_cell_measurement_temperature    293(2)
_cell_volume                     4150(3)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0668
_diffrn_reflns_av_sigmaI/netI    0.1020
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            9537
_diffrn_reflns_theta_full        26.49
_diffrn_reflns_theta_max         26.49
_diffrn_reflns_theta_min         2.14
_exptl_absorpt_coefficient_mu    2.437
_exptl_absorpt_correction_T_max  1.154
_exptl_absorpt_correction_T_min  0.981
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2000)'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.749
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2212
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.460
_refine_diff_density_min         -0.687
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         4269
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.1021
_refine_ls_R_factor_gt           0.0529
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0456P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0980
_refine_ls_wR_factor_ref         0.1110
_reflns_number_gt                2800
_reflns_number_total             4269
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0348502si20030718_093054_2.cif
_cod_data_source_block           2
_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               4312527
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
La1 La 0.0000 0.92998(5) 0.2500 0.02356(16) Uani 1 2 d S . .
Fe1 Fe 0.2500 0.7500 0.5000 0.0210(3) Uani 1 2 d S . .
Cu1 Cu 0.11587(4) 0.77180(8) 0.61159(5) 0.0414(2) Uani 1 1 d . . .
N3 N 0.0828(2) 0.9358(5) 0.5427(3) 0.0380(13) Uani 1 1 d . . .
C3 C 0.1383(4) 0.4853(8) 0.6381(5) 0.074(3) Uani 1 1 d . . .
H3A H 0.1093 0.4485 0.6451 0.089 Uiso 1 1 calc R . .
H3B H 0.1748 0.4292 0.6730 0.089 Uiso 1 1 calc R . .
C13 C 0.2231(2) 0.5658(7) 0.4820(4) 0.0295(14) Uani 1 1 d . . .
C11 C 0.1654(3) 0.8100(6) 0.4085(4) 0.0277(14) Uani 1 1 d . . .
N4 N 0.0682(2) 0.6879(5) 0.4929(3) 0.0325(13) Uani 1 1 d . . .
O2 O 0.02587(19) 1.0036(4) 0.3952(3) 0.0398(11) Uani 1 1 d . . .
C9 C 0.0498(3) 0.9162(6) 0.4570(4) 0.0308(14) Uani 1 1 d . . .
N11 N 0.1158(2) 0.8478(5) 0.3545(3) 0.0387(14) Uani 1 1 d . . .
N13 N 0.2088(3) 0.4581(6) 0.4726(4) 0.0526(17) Uani 1 1 d . . .
C12 C 0.2607(3) 0.7256(6) 0.4094(4) 0.0299(15) Uani 1 1 d . . .
O1 O 0.00568(18) 0.7503(4) 0.3436(3) 0.0355(11) Uani 1 1 d . . .
N2 N 0.1643(3) 0.8574(6) 0.7319(4) 0.0602(19) Uani 1 1 d . . .
H2C H 0.1335 0.8558 0.7362 0.072 Uiso 1 1 calc R . .
C10 C 0.0400(3) 0.7730(6) 0.4283(4) 0.0295(14) Uani 1 1 d . . .
N12 N 0.2659(3) 0.7088(6) 0.3554(4) 0.0504(16) Uani 1 1 d . . .
C4 C 0.1902(4) 0.6289(9) 0.7741(5) 0.070(3) Uani 1 1 d . . .
H4A H 0.2291 0.5812 0.8065 0.084 Uiso 1 1 calc R . .
H4B H 0.1670 0.5914 0.7918 0.084 Uiso 1 1 calc R . .
C6 C 0.1732(4) 0.9931(8) 0.7413(5) 0.060(2) Uani 1 1 d . . .
H6A H 0.2140 1.0090 0.7586 0.072 Uiso 1 1 calc R . .
H6B H 0.1759 1.0182 0.7927 0.072 Uiso 1 1 calc R . .
N1 N 0.1564(3) 0.6068(6) 0.6814(4) 0.0617(19) Uani 1 1 d . . .
H1C H 0.1899 0.6150 0.6833 0.074 Uiso 1 1 calc R . .
C1 C 0.0652(3) 0.5481(7) 0.4726(5) 0.0505(19) Uani 1 1 d . . .
H1A H 0.0246 0.5149 0.4484 0.061 Uiso 1 1 calc R . .
H1B H 0.0692 0.5390 0.4259 0.061 Uiso 1 1 calc R . .
C5 C 0.2038(3) 0.7664(8) 0.8028(5) 0.055(2) Uani 1 1 d . . .
H5A H 0.2000 0.7794 0.8495 0.066 Uiso 1 1 calc R . .
H5B H 0.2464 0.7851 0.8289 0.066 Uiso 1 1 calc R . .
C2 C 0.1118(5) 0.4660(9) 0.5484(5) 0.100(4) Uani 1 1 d . . .
H2A H 0.0944 0.3774 0.5335 0.120 Uiso 1 1 calc R . .
H2B H 0.1463 0.4627 0.5473 0.120 Uiso 1 1 calc R . .
O1W O 0.06951(19) 1.1293(5) 0.2981(3) 0.0509(13) Uani 1 1 d . . .
O2W O 0.1696(2) 0.1888(5) 0.4668(4) 0.0626(15) Uani 1 1 d . . .
C8 C 0.0987(4) 1.0723(8) 0.5775(5) 0.061(2) Uani 1 1 d . . .
H8A H 0.1229 1.1118 0.5622 0.073 Uiso 1 1 calc R . .
H8B H 0.0606 1.1229 0.5468 0.073 Uiso 1 1 calc R . .
O3W O 0.0241(2) 0.7437(5) 0.6224(4) 0.0714(17) Uani 1 1 d . . .
O4W O -0.0799(3) 0.5466(8) 0.2410(4) 0.139(4) Uani 1 1 d . . .
C7 C 0.1326(5) 1.0843(8) 0.6721(5) 0.106(4) Uani 1 1 d . . .
H7A H 0.1568 1.1648 0.6890 0.127 Uiso 1 1 calc R . .
H7B H 0.1016 1.1037 0.6791 0.127 Uiso 1 1 calc R . .
O5W O 0.0000 1.3793(11) 0.2500 0.205(8) 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'
La La -0.2871 2.4523 '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 La1 O1 86.0(2) 2 . ?
O1 La1 O2 64.88(14) 2 2 ?
O1 La1 O2 149.31(14) . 2 ?
O1 La1 O2 149.31(14) 2 . ?
O1 La1 O2 64.88(14) . . ?
O2 La1 O2 145.4(2) 2 . ?
O1 La1 O1W 122.15(15) 2 . ?
O1 La1 O1W 129.32(13) . . ?
O2 La1 O1W 77.64(14) 2 . ?
O2 La1 O1W 74.92(15) . . ?
O1 La1 O1W 129.32(13) 2 2 ?
O1 La1 O1W 122.15(15) . 2 ?
O2 La1 O1W 74.92(15) 2 2 ?
O2 La1 O1W 77.64(14) . 2 ?
O1W La1 O1W 74.4(2) . 2 ?
O1 La1 N11 74.35(15) 2 2 ?
O1 La1 N11 78.92(15) . 2 ?
O2 La1 N11 83.88(15) 2 2 ?
O2 La1 N11 107.13(15) . 2 ?
O1W La1 N11 144.62(15) . 2 ?
O1W La1 N11 71.81(15) 2 2 ?
O1 La1 N11 78.92(15) 2 . ?
O1 La1 N11 74.35(15) . . ?
O2 La1 N11 107.13(15) 2 . ?
O2 La1 N11 83.88(15) . . ?
O1W La1 N11 71.81(15) . . ?
O1W La1 N11 144.62(16) 2 . ?
N11 La1 N11 143.2(2) 2 . ?
C11 Fe1 C11 180.0(3) 7_566 . ?
C11 Fe1 C12 90.9(2) 7_566 7_566 ?
C11 Fe1 C12 89.1(2) . 7_566 ?
C11 Fe1 C12 89.1(2) 7_566 . ?
C11 Fe1 C12 90.9(2) . . ?
C12 Fe1 C12 180.00(8) 7_566 . ?
C11 Fe1 C13 91.5(2) 7_566 7_566 ?
C11 Fe1 C13 88.5(2) . 7_566 ?
C12 Fe1 C13 88.8(2) 7_566 7_566 ?
C12 Fe1 C13 91.2(2) . 7_566 ?
C11 Fe1 C13 88.5(2) 7_566 . ?
C11 Fe1 C13 91.5(2) . . ?
C12 Fe1 C13 91.2(2) 7_566 . ?
C12 Fe1 C13 88.8(2) . . ?
C13 Fe1 C13 180.000(1) 7_566 . ?
N3 Cu1 N4 84.2(2) . . ?
N3 Cu1 N1 174.3(3) . . ?
N4 Cu1 N1 95.6(2) . . ?
N3 Cu1 N2 95.6(2) . . ?
N4 Cu1 N2 179.8(3) . . ?
N1 Cu1 N2 84.5(2) . . ?
C9 N3 C8 119.1(6) . . ?
C9 N3 Cu1 112.4(4) . . ?
C8 N3 Cu1 127.7(4) . . ?
N1 C3 C2 124.9(8) . . ?
N1 C3 H3A 106.1 . . ?
C2 C3 H3A 106.1 . . ?
N1 C3 H3B 106.1 . . ?
C2 C3 H3B 106.1 . . ?
H3A C3 H3B 106.3 . . ?
N13 C13 Fe1 178.4(5) . . ?
N11 C11 Fe1 178.7(6) . . ?
C10 N4 C1 119.7(5) . . ?
C10 N4 Cu1 112.3(4) . . ?
C1 N4 Cu1 127.9(4) . . ?
C9 O2 La1 116.0(4) . . ?
O2 C9 N3 127.3(6) . . ?
O2 C9 C10 117.3(5) . . ?
N3 C9 C10 115.4(6) . . ?
C11 N11 La1 171.0(5) . . ?
N12 C12 Fe1 178.3(6) . . ?
C10 O1 La1 116.0(4) . . ?
C6 N2 C5 123.5(6) . . ?
C6 N2 Cu1 121.1(5) . . ?
C5 N2 Cu1 112.0(5) . . ?
C6 N2 H2C 96.2 . . ?
C5 N2 H2C 96.2 . . ?
Cu1 N2 H2C 96.2 . . ?
O1 C10 N4 127.6(6) . . ?
O1 C10 C9 116.9(5) . . ?
N4 C10 C9 115.5(6) . . ?
N1 C4 C5 115.8(7) . . ?
N1 C4 H4A 108.3 . . ?
C5 C4 H4A 108.3 . . ?
N1 C4 H4B 108.3 . . ?
C5 C4 H4B 108.3 . . ?
H4A C4 H4B 107.4 . . ?
N2 C6 C7 123.6(7) . . ?
N2 C6 H6A 106.4 . . ?
C7 C6 H6A 106.4 . . ?
N2 C6 H6B 106.4 . . ?
C7 C6 H6B 106.4 . . ?
H6A C6 H6B 106.5 . . ?
C3 N1 C4 126.6(7) . . ?
C3 N1 Cu1 120.3(5) . . ?
C4 N1 Cu1 111.0(5) . . ?
C3 N1 H1C 94.7 . . ?
C4 N1 H1C 94.7 . . ?
Cu1 N1 H1C 94.7 . . ?
C2 C1 N4 115.2(6) . . ?
C2 C1 H1A 108.5 . . ?
N4 C1 H1A 108.5 . . ?
C2 C1 H1B 108.5 . . ?
N4 C1 H1B 108.5 . . ?
H1A C1 H1B 107.5 . . ?
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 126.7(8) . . ?
C3 C2 H2A 105.6 . . ?
C1 C2 H2A 105.6 . . ?
C3 C2 H2B 105.6 . . ?
C1 C2 H2B 105.6 . . ?
H2A C2 H2B 106.1 . . ?
La1 O1W H100 119.5 . . ?
La1 O1W H101 107.6 . . ?
H100 O1W H101 124.7 . . ?
H201 O2W H200 103.6 . . ?
C7 C8 N3 115.0(7) . . ?
C7 C8 H8A 108.5 . . ?
N3 C8 H8A 108.5 . . ?
C7 C8 H8B 108.5 . . ?
N3 C8 H8B 108.5 . . ?
H8A C8 H8B 107.5 . . ?
H300 O3W H301 89.3 . . ?
H401 O4W H400 106.1 . . ?
C6 C7 C8 129.3(9) . . ?
C6 C7 H7A 105.0 . . ?
C8 C7 H7A 105.0 . . ?
C6 C7 H7B 105.0 . . ?
C8 C7 H7B 105.0 . . ?
H7A C7 H7B 105.8 . . ?
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
La1 O1 2.480(4) 2 ?
La1 O1 2.480(4) . ?
La1 O2 2.498(4) 2 ?
La1 O2 2.498(4) . ?
La1 O1W 2.526(5) . ?
La1 O1W 2.526(4) 2 ?
La1 N11 2.629(5) 2 ?
La1 N11 2.629(5) . ?
Fe1 C11 1.939(6) 7_566 ?
Fe1 C11 1.939(6) . ?
Fe1 C12 1.946(6) 7_566 ?
Fe1 C12 1.946(6) . ?
Fe1 C13 1.952(7) 7_566 ?
Fe1 C13 1.952(7) . ?
Cu1 N3 1.947(5) . ?
Cu1 N4 1.954(5) . ?
Cu1 N1 1.982(6) . ?
Cu1 N2 1.984(6) . ?
N3 C9 1.290(7) . ?
N3 C8 1.472(9) . ?
C3 N1 1.385(9) . ?
C3 C2 1.386(11) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C13 N13 1.131(8) . ?
C11 N11 1.146(7) . ?
N4 C10 1.287(7) . ?
N4 C1 1.452(8) . ?
O2 C9 1.274(7) . ?
C9 C10 1.508(9) . ?
C12 N12 1.140(7) . ?
O1 C10 1.278(7) . ?
N2 C6 1.384(9) . ?
N2 C5 1.416(8) . ?
N2 H2C 0.9100 . ?
C4 N1 1.403(9) . ?
C4 C5 1.451(10) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C6 C7 1.410(10) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
N1 H1C 0.9100 . ?
C1 C2 1.447(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 0.7967 . ?
O1W H101 0.7786 . ?
O2W H201 0.8429 . ?
O2W H200 0.8639 . ?
C8 C7 1.421(10) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
O3W H300 0.9280 . ?
O3W H301 0.9027 . ?
O4W H401 0.8563 . ?
O4W H400 0.8977 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
O5W H500 0.8199 . ?
