#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:11:23 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179316 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/13/4321320.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_4321320
loop_
_publ_author_name
'Yong Cui'
'Gang Chen'
'Jin Ren'
'Yitai Qian'
'Jinshun Huang'
_publ_section_title
;
 Syntheses, Structures and Magnetic Behaviors of Di- and Trinuclear
 Pivalate Complexes Containing Both Cobalt(II) and Lanthanide(III) Ions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4165
_journal_page_last               4168
_journal_paper_doi               10.1021/ic000230e
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C48 H68 Co2 Gd N3 O15'
_chemical_formula_weight         1202.16
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 115.79(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.282(5)
_cell_length_b                   11.644(2)
_cell_length_c                   24.301(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.99
_cell_measurement_theta_min      1.86
_cell_volume                     5677(2)
_computing_cell_refinement       'PSi SCANS'
_computing_data_collection       'Enraf-nonius CAD4'
_computing_data_reduction        'Siemens XPREP'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-nonius CAD4'
_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  0.0745
_diffrn_reflns_av_sigmaI/netI    0.1040
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            10843
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         1.86
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    1.794
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  .7832
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_description       prism
_exptl_crystal_F_000             2460
_exptl_crystal_size_max          .20
_exptl_crystal_size_mid          .15
_exptl_crystal_size_min          .15
_refine_diff_density_max         0.807
_refine_diff_density_min         -0.444
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_gt    1.063
_refine_ls_goodness_of_fit_ref   0.956
_refine_ls_matrix_type           full
_refine_ls_number_parameters     303
_refine_ls_number_reflns         5571
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.019
_refine_ls_restrained_S_obs      1.105
_refine_ls_R_factor_all          0.1099
_refine_ls_R_factor_gt           0.0558
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0746P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1315
_refine_ls_wR_factor_ref         0.1553
_reflns_number_gt                3557
_reflns_number_total             5572
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000230e_3.cif
_cod_data_source_block           4
_cod_original_cell_volume        5676.9(20)
_cod_database_code               4321320
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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Gd Gd 0.5000 0.07429(5) 0.2500 0.0421(2) Uani 1 d S .
Co Co 0.47958(5) 0.19884(9) 0.08797(4) 0.0524(3) Uani 1 d . .
O1 O 0.5380(4) -0.1156(6) 0.2334(3) 0.091(2) Uani 1 d . .
O2 O 0.4806(8) -0.2754(13) 0.2446(9) 0.107(5) Uiso 0.50 d P .
O11 O 0.4254(3) 0.0131(6) 0.1526(2) 0.086(2) Uani 1 d . .
O12 O 0.4173(3) 0.0712(6) 0.0645(3) 0.080(2) Uani 1 d . .
O21 O 0.4428(4) 0.2357(6) 0.1964(3) 0.088(2) Uani 1 d . .
O22 O 0.4491(3) 0.3241(5) 0.1208(3) 0.077(2) Uani 1 d . .
O31 O 0.5708(3) 0.1058(5) 0.2055(3) 0.073(2) Uani 1 d . .
O32 O 0.5742(3) 0.1594(6) 0.1210(3) 0.075(2) Uani 1 d . .
N1 N 0.5000 -0.1713(9) 0.2500 0.109(6) Uani 1 d S .
N2 N 0.4659(4) 0.2472(6) 0.0002(3) 0.061(2) Uani 1 d . .
C11 C 0.3972(5) 0.0132(7) 0.0969(3) 0.064(2) Uani 1 d . .
C12 C 0.3347(6) -0.0590(10) 0.0646(4) 0.103(4) Uani 1 d D .
C13 C 0.3491(13) -0.1754(19) 0.0997(11) 0.106(7) Uiso 0.50 d PD 1
C14 C 0.2733(17) -0.0024(37) 0.0619(21) 0.157(17) Uiso 0.50 d PD 1
C15 C 0.3154(12) -0.0729(21) -0.0035(8) 0.088(6) Uiso 0.50 d PD 1
C13A C 0.3165(11) -0.1330(19) 0.1070(9) 0.085(6) Uiso 0.50 d PD 2
C14A C 0.2796(16) 0.0369(30) 0.0496(19) 0.137(14) Uiso 0.50 d PD 2
C15A C 0.3450(18) -0.1217(30) 0.0113(14) 0.147(12) Uiso 0.50 d PD 2
C21 C 0.4293(4) 0.3149(7) 0.1624(4) 0.060(2) Uani 1 d . .
C22 C 0.3834(5) 0.4102(8) 0.1650(4) 0.088(3) Uani 1 d D .
C23 C 0.4098(14) 0.5251(19) 0.1469(11) 0.102(8) Uiso 0.50 d PD 1
C24 C 0.3138(13) 0.3964(30) 0.1173(14) 0.132(13) Uiso 0.50 d PD 1
C25 C 0.4012(10) 0.4417(17) 0.2320(7) 0.066(5) Uiso 0.50 d PD 1
C23A C 0.3736(16) 0.5181(20) 0.1307(12) 0.109(9) Uiso 0.50 d PD 2
C24A C 0.3123(10) 0.3494(23) 0.1262(10) 0.085(7) Uiso 0.50 d PD 2
C25A C 0.3801(10) 0.4000(18) 0.2283(7) 0.073(6) Uiso 0.50 d PD 2
C31 C 0.6011(4) 0.1207(7) 0.1745(4) 0.058(2) Uani 1 d . .
C32 C 0.6750(5) 0.0881(10) 0.1999(4) 0.086(3) Uani 1 d D .
C33 C 0.6979(13) 0.0346(23) 0.2637(10) 0.112(8) Uiso 0.50 d PD 1
C34 C 0.6734(13) -0.0279(19) 0.1650(12) 0.107(8) Uiso 0.50 d PD 1
C35 C 0.7184(14) 0.1890(22) 0.1959(14) 0.124(10) Uiso 0.50 d PD 1
C33A C 0.7153(17) 0.1365(34) 0.2664(12) 0.170(13) Uiso 0.50 d PD 2
C34A C 0.6857(17) -0.0374(19) 0.2106(17) 0.145(11) Uiso 0.50 d PD 2
C35A C 0.7096(11) 0.1433(22) 0.1652(11) 0.096(7) Uiso 0.50 d PD 2
C41 C 0.4837(7) 0.1654(10) -0.0273(5) 0.100(4) Uani 1 d . .
H41A H 0.5010(7) 0.0976(10) -0.0061(5) 0.120 Uiso 1 calc R .
C42 C 0.4780(8) 0.1756(12) -0.0869(5) 0.135(6) Uani 1 d . .
H42A H 0.4922(8) 0.1166(12) -0.1041(5) 0.162 Uiso 1 calc R .
C43 C 0.4518(7) 0.2706(13) -0.1183(5) 0.117(5) Uani 1 d . .
H43A H 0.4451(7) 0.2763(13) -0.1587(5) 0.140 Uiso 1 calc R .
C44 C 0.4346(5) 0.3607(9) -0.0914(4) 0.074(3) Uani 1 d . .
C45 C 0.4110(7) 0.4666(12) -0.1206(6) 0.108(4) Uani 1 d . .
H45A H 0.4072(7) 0.4787(12) -0.1598(6) 0.129 Uiso 1 calc R .
C46 C 0.3944(6) 0.5484(11) -0.0927(6) 0.110(4) Uani 1 d . .
H46A H 0.3781(6) 0.6174(11) -0.1130(6) 0.132 Uiso 1 calc R .
C47 C 0.4006(6) 0.5349(9) -0.0334(6) 0.094(3) Uani 1 d . .
H47A H 0.3886(6) 0.5946(9) -0.0147(6) 0.113 Uiso 1 calc R .
C48 C 0.4238(5) 0.4355(8) -0.0032(4) 0.072(2) Uani 1 d . .
H48A H 0.4284(5) 0.4272(8) 0.0365(4) 0.086 Uiso 1 calc R .
C49 C 0.4408(4) 0.3457(7) -0.0310(3) 0.058(2) Uani 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'
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'
Co Co 0.3494 0.9721 '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'
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
O31 Gd O31 161.6(3) . 2_655 ?
O31 Gd O21 79.2(2) . 2_655 ?
O31 Gd O21 85.9(2) 2_655 2_655 ?
O31 Gd O21 85.9(2) . . ?
O31 Gd O21 79.2(2) 2_655 . ?
O21 Gd O21 72.2(4) 2_655 . ?
O31 Gd O11 84.5(2) . . ?
O31 Gd O11 101.2(2) 2_655 . ?
O21 Gd O11 142.1(2) 2_655 . ?
O21 Gd O11 72.8(3) . . ?
O31 Gd O11 101.2(2) . 2_655 ?
O31 Gd O11 84.5(2) 2_655 2_655 ?
O21 Gd O11 72.8(3) 2_655 2_655 ?
O21 Gd O11 142.1(2) . 2_655 ?
O11 Gd O11 144.5(3) . 2_655 ?
O31 Gd O1 125.2(2) . 2_655 ?
O31 Gd O1 73.2(2) 2_655 2_655 ?
O21 Gd O1 141.0(2) 2_655 2_655 ?
O21 Gd O1 132.3(3) . 2_655 ?
O11 Gd O1 75.4(2) . 2_655 ?
O11 Gd O1 72.8(3) 2_655 2_655 ?
O31 Gd O1 73.2(2) . . ?
O31 Gd O1 125.2(2) 2_655 . ?
O21 Gd O1 132.3(3) 2_655 . ?
O21 Gd O1 141.0(2) . . ?
O11 Gd O1 72.8(3) . . ?
O11 Gd O1 75.4(2) 2_655 . ?
O1 Gd O1 52.3(4) 2_655 . ?
O31 Gd N1 99.2(2) . . ?
O31 Gd N1 99.2(2) 2_655 . ?
O21 Gd N1 143.9(2) 2_655 . ?
O21 Gd N1 143.9(2) . . ?
O11 Gd N1 72.2(2) . . ?
O11 Gd N1 72.2(2) 2_655 . ?
O1 Gd N1 26.1(2) 2_655 . ?
O1 Gd N1 26.1(2) . . ?
O31 Gd Co 44.89(15) . . ?
O31 Gd Co 126.4(2) 2_655 . ?
O21 Gd Co 93.3(2) 2_655 . ?
O21 Gd Co 50.27(14) . . ?
O11 Gd Co 52.5(2) . . ?
O11 Gd Co 145.9(2) 2_655 . ?
O1 Gd Co 125.59(15) 2_655 . ?
O1 Gd Co 93.67(15) . . ?
N1 Gd Co 111.08(2) . . ?
O22 Co O12 111.5(3) . . ?
O22 Co O32 121.3(3) . . ?
O12 Co O32 116.5(3) . . ?
O22 Co N2 107.3(3) . . ?
O12 Co N2 97.9(3) . . ?
O32 Co N2 97.7(3) . . ?
O22 Co Gd 77.1(2) . . ?
O12 Co Gd 77.0(2) . . ?
O32 Co Gd 82.6(2) . . ?
N2 Co Gd 174.3(2) . . ?
N1 O1 Gd 94.8(6) . . ?
O2 O2 N1 72.0(7) 2_655 . ?
C11 O11 Gd 157.0(6) . . ?
C11 O12 Co 129.0(5) . . ?
C21 O21 Gd 158.4(6) . . ?
C21 O22 Co 125.0(5) . . ?
C31 O31 Gd 171.4(6) . . ?
C31 O32 Co 116.9(5) . . ?
O1 N1 O1 118.2(10) . 2_655 ?
O1 N1 O2 106.1(9) . 2_655 ?
O1 N1 O2 134.4(10) 2_655 2_655 ?
O1 N1 O2 134.4(10) . . ?
O1 N1 O2 106.1(9) 2_655 . ?
O2 N1 O2 36.0(14) 2_655 . ?
O1 N1 Gd 59.1(5) . . ?
O1 N1 Gd 59.1(5) 2_655 . ?
O2 N1 Gd 162.0(7) 2_655 . ?
O2 N1 Gd 162.0(7) . . ?
C41 N2 C49 118.0(7) . . ?
C41 N2 Co 112.3(6) . . ?
C49 N2 Co 129.7(5) . . ?
O11 C11 O12 123.0(8) . . ?
O11 C11 C12 119.0(8) . . ?
O12 C11 C12 118.0(7) . . ?
C14 C12 C11 113.2(21) . . ?
C11 C12 C13A 114.7(10) . . ?
C14 C12 C15 100.3(21) . . ?
C11 C12 C15 112.3(11) . . ?
C14 C12 C13 112.0(22) . . ?
C11 C12 C13 106.0(12) . . ?
C15 C12 C13 113.2(15) . . ?
C11 C12 C14A 100.0(17) . . ?
C13A C12 C14A 98.5(20) . . ?
C11 C12 C15A 104.4(15) . . ?
C13A C12 C15A 117.8(18) . . ?
C14A C12 C15A 120.7(21) . . ?
O21 C21 O22 123.2(8) . . ?
O21 C21 C22 120.5(8) . . ?
O22 C21 C22 116.2(7) . . ?
C23A C22 C21 122.2(13) . . ?
C24 C22 C21 112.2(16) . . ?
C24 C22 C25 123.5(18) . . ?
C21 C22 C25 110.3(9) . . ?
C23A C22 C25A 124.0(15) . . ?
C21 C22 C25A 107.6(10) . . ?
C24 C22 C23 105.0(18) . . ?
C21 C22 C23 105.3(12) . . ?
C25 C22 C23 97.8(12) . . ?
C23A C22 C24A 100.3(16) . . ?
C21 C22 C24A 99.3(11) . . ?
C25A C22 C24A 95.0(12) . . ?
O31 C31 O32 123.1(7) . . ?
O31 C31 C32 120.1(8) . . ?
O32 C31 C32 116.7(7) . . ?
C34A C32 C35A 115.7(18) . . ?
C34A C32 C31 112.1(16) . . ?
C35A C32 C31 113.0(11) . . ?
C31 C32 C33 109.4(12) . . ?
C31 C32 C35 112.2(13) . . ?
C33 C32 C35 115.3(17) . . ?
C34A C32 C33A 101.3(20) . . ?
C35A C32 C33A 102.7(18) . . ?
C31 C32 C33A 110.9(15) . . ?
C31 C32 C34 103.0(12) . . ?
C33 C32 C34 96.6(15) . . ?
C35 C32 C34 118.8(16) . . ?
N2 C41 C42 123.3(10) . . ?
C43 C42 C41 119.0(11) . . ?
C42 C43 C44 120.4(9) . . ?
C43 C44 C45 123.3(10) . . ?
C43 C44 C49 118.2(9) . . ?
C45 C44 C49 118.4(10) . . ?
C46 C45 C44 120.3(11) . . ?
C45 C46 C47 121.9(11) . . ?
C48 C47 C46 120.0(11) . . ?
C47 C48 C49 120.3(9) . . ?
N2 C49 C48 120.0(7) . . ?
N2 C49 C44 120.9(8) . . ?
C48 C49 C44 119.0(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
Gd O31 2.299(5) . ?
Gd O31 2.299(5) 2_655 ?
Gd O21 2.326(6) 2_655 ?
Gd O21 2.326(6) . ?
Gd O11 2.334(5) . ?
Gd O11 2.334(5) 2_655 ?
Gd O1 2.463(7) 2_655 ?
Gd O1 2.463(7) . ?
Gd N1 2.860(11) . ?
Gd Co 4.0317(12) . ?
Co O22 1.922(5) . ?
Co O12 1.942(6) . ?
Co O32 1.956(6) . ?
Co N2 2.097(6) . ?
O1 N1 1.264(8) . ?
O2 O2 0.79(3) 2_655 ?
O2 N1 1.27(2) . ?
O11 C11 1.221(9) . ?
O12 C11 1.258(10) . ?
O21 C21 1.185(9) . ?
O22 C21 1.272(9) . ?
O31 C31 1.220(9) . ?
O32 C31 1.255(9) . ?
N1 O1 1.264(8) 2_655 ?
N1 O2 1.27(2) 2_655 ?
N2 C41 1.319(11) . ?
N2 C49 1.354(10) . ?
C11 C12 1.520(13) . ?
C12 C14 1.49(2) . ?
C12 C13A 1.53(2) . ?
C12 C15 1.53(2) . ?
C12 C13 1.56(2) . ?
C12 C14A 1.58(2) . ?
C12 C15A 1.59(2) . ?
C21 C22 1.529(11) . ?
C22 C23A 1.47(2) . ?
C22 C24 1.49(2) . ?
C22 C25 1.54(2) . ?
C22 C25A 1.58(2) . ?
C22 C23 1.60(2) . ?
C22 C24A 1.61(2) . ?
C31 C32 1.534(12) . ?
C32 C34A 1.49(2) . ?
C32 C35A 1.51(2) . ?
C32 C33 1.54(2) . ?
C32 C35 1.55(2) . ?
C32 C33A 1.57(2) . ?
C32 C34 1.59(2) . ?
C41 C42 1.402(13) . ?
C42 C43 1.33(2) . ?
C43 C44 1.377(15) . ?
C44 C45 1.405(15) . ?
C44 C49 1.422(11) . ?
C45 C46 1.31(2) . ?
C46 C47 1.40(2) . ?
C47 C48 1.347(12) . ?
C48 C49 1.386(12) . ?
