#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:40:34 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179122 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/84/4308453.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_4308453
loop_
_publ_author_name
'Jie Zhang'
'Xigeng Zhou'
'Ruifang Cai'
'Linhong Weng'
_publ_section_title
;
Reactivity of Organolanthanide and Organolithium Complexes Containing the
Guanidinate Ligands toward Isocyanate or Carbodiimide: Synthesis and
Crystal Structures
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              716
_journal_page_last               722
_journal_paper_doi               10.1021/ic048683x
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C52 H70 Gd2 N8 O4'
_chemical_formula_weight         1185.66
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                97.327(4)
_cell_angle_beta                 92.531(4)
_cell_angle_gamma                100.162(4)
_cell_formula_units_Z            1
_cell_length_a                   8.865(3)
_cell_length_b                   10.953(3)
_cell_length_c                   13.984(4)
_cell_measurement_reflns_used    902
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.164
_cell_measurement_theta_min      2.564
_cell_volume                     1322.5(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_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  0.0163
_diffrn_reflns_av_sigmaI/netI    0.0267
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5541
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.47
_diffrn_standards_decay_%        1.99
_exptl_absorpt_coefficient_mu    2.535
_exptl_absorpt_correction_T_max  0.7023
_exptl_absorpt_correction_T_min  0.5168
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             598
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.085
_refine_diff_density_min         -0.544
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         4580
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0325
_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)+(0.0515P)²+2.1211P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0843
_refine_ls_wR_factor_ref         0.0875
_reflns_number_gt                4250
_reflns_number_total             4580
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048683xsi20041217_110608.cif
_cod_data_source_block           f40302a
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        1322.5(6)
_cod_database_code               4308453
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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 0.42756(2) -0.094072(19) 0.371633(15) 0.03609(10) Uani 1 1 d . . .
N1 N 0.6092(4) 0.0669(4) 0.3071(3) 0.0404(9) Uani 1 1 d . . .
N2 N 0.7737(5) 0.2340(4) 0.4124(3) 0.0447(9) Uani 1 1 d . . .
N3 N 0.6925(6) 0.3708(4) 0.3120(4) 0.0568(11) Uani 1 1 d . . .
N4 N 0.9503(5) 0.3873(4) 0.3594(4) 0.0598(12) Uani 1 1 d . . .
O1 O 0.5851(4) 0.0913(3) 0.4631(2) 0.0416(7) Uani 1 1 d . . .
C1 C 0.5972(9) -0.2722(6) 0.4010(6) 0.0768(19) Uani 1 1 d . . .
H1A H 0.6530 -0.2775 0.4620 0.092 Uiso 1 1 calc R . .
C2 C 0.6617(9) -0.2171(6) 0.3237(8) 0.090(3) Uani 1 1 d . . .
H2A H 0.7696 -0.1784 0.3211 0.108 Uiso 1 1 calc R . .
C3 C 0.5525(15) -0.2475(9) 0.2463(6) 0.103(3) Uani 1 1 d . . .
H3A H 0.5707 -0.2370 0.1789 0.123 Uiso 1 1 calc R . .
C4 C 0.4263(12) -0.3252(8) 0.2781(9) 0.110(3) Uani 1 1 d . . .
H4A H 0.3405 -0.3763 0.2362 0.132 Uiso 1 1 calc R . .
C5 C 0.4552(10) -0.3340(6) 0.3720(7) 0.086(2) Uani 1 1 d . . .
H5A H 0.3928 -0.3926 0.4084 0.103 Uiso 1 1 calc R . .
C6 C 0.1492(9) -0.1599(9) 0.2756(8) 0.099(3) Uani 1 1 d . . .
H6A H 0.1125 -0.2408 0.2355 0.119 Uiso 1 1 calc R . .
C7 C 0.1162(7) -0.1330(8) 0.3672(7) 0.080(2) Uani 1 1 d . . .
H7A H 0.0525 -0.1907 0.4037 0.096 Uiso 1 1 calc R . .
C8 C 0.1634(8) -0.0074(9) 0.3961(6) 0.087(2) Uani 1 1 d . . .
H8A H 0.1364 0.0408 0.4547 0.104 Uiso 1 1 calc R . .
C9 C 0.2268(7) 0.0426(7) 0.3137(9) 0.097(3) Uani 1 1 d . . .
H9A H 0.2501 0.1313 0.3054 0.117 Uiso 1 1 calc R . .
C10 C 0.2156(10) -0.0575(12) 0.2420(6) 0.100(3) Uani 1 1 d . . .
H10A H 0.2317 -0.0511 0.1738 0.120 Uiso 1 1 calc R . .
C11 C 0.6572(5) 0.1339(4) 0.3904(3) 0.0363(9) Uani 1 1 d . . .
C12 C 0.8019(6) 0.3252(5) 0.3604(4) 0.0482(12) Uani 1 1 d . . .
C13 C 0.9879(9) 0.5211(6) 0.3588(6) 0.084(2) Uani 1 1 d . . .
H13A H 0.8978 0.5511 0.3385 0.126 Uiso 1 1 calc R . .
H13B H 1.0663 0.5394 0.3148 0.126 Uiso 1 1 calc R . .
H13C H 1.0244 0.5617 0.4226 0.126 Uiso 1 1 calc R . .
C14 C 1.0764(7) 0.3270(7) 0.3880(6) 0.080(2) Uani 1 1 d . . .
H14A H 1.0396 0.2388 0.3858 0.119 Uiso 1 1 calc R . .
H14B H 1.1159 0.3623 0.4525 0.119 Uiso 1 1 calc R . .
H14C H 1.1566 0.3403 0.3445 0.119 Uiso 1 1 calc R . .
C15 C 0.5339(7) 0.3471(6) 0.3349(5) 0.0696(17) Uani 1 1 d . . .
H15A H 0.5261 0.3120 0.3944 0.104 Uiso 1 1 calc R . .
H15B H 0.4744 0.2894 0.2839 0.104 Uiso 1 1 calc R . .
H15C H 0.4957 0.4243 0.3417 0.104 Uiso 1 1 calc R . .
C16 C 0.7213(10) 0.4244(6) 0.2216(5) 0.084(2) Uani 1 1 d . . .
H16A H 0.8293 0.4370 0.2122 0.126 Uiso 1 1 calc R . .
H16B H 0.6872 0.5032 0.2254 0.126 Uiso 1 1 calc R . .
H16C H 0.6663 0.3680 0.1682 0.126 Uiso 1 1 calc R . .
C17 C 0.6849(6) 0.0835(4) 0.2210(3) 0.0445(11) Uani 1 1 d . . .
C18 C 0.6017(7) 0.1016(5) 0.1397(4) 0.0590(14) Uani 1 1 d . . .
H18A H 0.4985 0.1073 0.1425 0.071 Uiso 1 1 calc R . .
C19 C 0.6737(8) 0.1111(7) 0.0532(4) 0.0732(18) Uani 1 1 d . . .
H19A H 0.6177 0.1228 -0.0017 0.088 Uiso 1 1 calc R . .
C20 C 0.8239(8) 0.1036(7) 0.0486(5) 0.079(2) Uani 1 1 d . . .
H20A H 0.8712 0.1110 -0.0090 0.094 Uiso 1 1 calc R . .
C21 C 0.9064(8) 0.0849(7) 0.1291(5) 0.0766(19) Uani 1 1 d . . .
H21A H 1.0095 0.0791 0.1260 0.092 Uiso 1 1 calc R . .
C22 C 0.8373(7) 0.0746(6) 0.2141(4) 0.0588(14) Uani 1 1 d . . .
H22A H 0.8942 0.0615 0.2681 0.071 Uiso 1 1 calc R . .
O2 O 0.168(2) 0.4515(17) 0.0662(16) 0.355(10) Uiso 1 1 d D . .
C23 C 0.231(2) 0.3638(18) 0.1229(12) 0.217(7) Uiso 1 1 d D . .
H23A H 0.3183 0.4066 0.1662 0.261 Uiso 1 1 calc R . .
H23B H 0.1539 0.3199 0.1595 0.261 Uiso 1 1 calc R . .
C24 C 0.278(3) 0.2782(18) 0.0431(16) 0.259(9) Uiso 1 1 d D . .
H24A H 0.1920 0.2183 0.0102 0.311 Uiso 1 1 calc R . .
H24B H 0.3576 0.2351 0.0642 0.311 Uiso 1 1 calc R . .
C25 C 0.337(3) 0.379(3) -0.016(3) 0.52(3) Uiso 1 1 d D . .
H25A H 0.3877 0.4583 0.0202 0.620 Uiso 1 1 calc R . .
H25B H 0.3912 0.3532 -0.0717 0.620 Uiso 1 1 calc R . .
C26 C 0.168(3) 0.360(3) -0.0305(16) 0.321(13) Uiso 1 1 d D . .
H26A H 0.1164 0.2749 -0.0279 0.385 Uiso 1 1 calc R . .
H26B H 0.1322 0.3912 -0.0876 0.385 Uiso 1 1 calc R . .
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'
Gd Gd -0.1653 3.9035 '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'
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 67.45(12) 2_656 . ?
O1 Gd1 N1 120.30(12) 2_656 . ?
O1 Gd1 N1 53.23(12) . . ?
O1 Gd1 C10 128.9(2) 2_656 . ?
O1 Gd1 C10 116.9(3) . . ?
N1 Gd1 C10 87.4(3) . . ?
O1 Gd1 C9 107.3(3) 2_656 . ?
O1 Gd1 C9 90.9(2) . . ?
N1 Gd1 C9 81.51(18) . . ?
C10 Gd1 C9 29.8(3) . . ?
O1 Gd1 C5 84.5(2) 2_656 . ?
O1 Gd1 C5 128.1(2) . . ?
N1 Gd1 C5 125.87(19) . . ?
C10 Gd1 C5 114.7(4) . . ?
C9 Gd1 C5 140.2(3) . . ?
O1 Gd1 C3 128.7(2) 2_656 . ?
O1 Gd1 C3 120.6(3) . . ?
N1 Gd1 C3 82.1(3) . . ?
C10 Gd1 C3 94.5(3) . . ?
C9 Gd1 C3 122.1(4) . . ?
C5 Gd1 C3 49.3(3) . . ?
O1 Gd1 C6 112.5(3) 2_656 . ?
O1 Gd1 C6 138.3(2) . . ?
N1 Gd1 C6 115.4(3) . . ?
C10 Gd1 C6 28.6(3) . . ?
C9 Gd1 C6 48.2(3) . . ?
C5 Gd1 C6 92.1(3) . . ?
C3 Gd1 C6 92.6(4) . . ?
O1 Gd1 C8 80.11(19) 2_656 . ?
O1 Gd1 C8 93.8(2) . . ?
N1 Gd1 C8 107.8(2) . . ?
C10 Gd1 C8 49.4(2) . . ?
C9 Gd1 C8 30.9(3) . . ?
C5 Gd1 C8 124.4(3) . . ?
C3 Gd1 C8 140.4(3) . . ?
C6 Gd1 C8 48.2(3) . . ?
O1 Gd1 C4 112.6(3) 2_656 . ?
O1 Gd1 C4 145.2(2) . . ?
N1 Gd1 C4 112.0(3) . . ?
C10 Gd1 C4 90.7(4) . . ?
C9 Gd1 C4 120.0(3) . . ?
C5 Gd1 C4 29.0(3) . . ?
C3 Gd1 C4 30.3(3) . . ?
C6 Gd1 C4 75.6(3) . . ?
C8 Gd1 C4 120.9(3) . . ?
O1 Gd1 C7 84.8(2) 2_656 . ?
O1 Gd1 C7 121.7(2) . . ?
N1 Gd1 C7 130.12(17) . . ?
C10 Gd1 C7 47.9(3) . . ?
C9 Gd1 C7 48.9(2) . . ?
C5 Gd1 C7 96.6(2) . . ?
C3 Gd1 C7 116.8(4) . . ?
C6 Gd1 C7 28.6(3) . . ?
C8 Gd1 C7 29.3(2) . . ?
C4 Gd1 C7 92.3(3) . . ?
O1 Gd1 C1 79.98(19) 2_656 . ?
O1 Gd1 C1 101.28(19) . . ?
N1 Gd1 C1 103.7(2) . . ?
C10 Gd1 C1 138.2(3) . . ?
C9 Gd1 C1 167.6(3) . . ?
C5 Gd1 C1 28.7(2) . . ?
C3 Gd1 C1 49.0(3) . . ?
C6 Gd1 C1 120.1(3) . . ?
C8 Gd1 C1 148.1(3) . . ?
C4 Gd1 C1 47.6(3) . . ?
C7 Gd1 C1 123.9(2) . . ?
C11 N1 C17 123.0(4) . . ?
C11 N1 Gd1 96.2(3) . . ?
C17 N1 Gd1 138.9(3) . . ?
C12 N2 C11 124.0(4) . . ?
C12 N3 C15 121.5(5) . . ?
C12 N3 C16 122.1(5) . . ?
C15 N3 C16 115.3(5) . . ?
C12 N4 C13 122.3(5) . . ?
C12 N4 C14 119.2(5) . . ?
C13 N4 C14 116.1(5) . . ?
C11 O1 Gd1 148.7(3) . 2_656 ?
C11 O1 Gd1 97.3(3) . . ?
Gd1 O1 Gd1 112.55(12) 2_656 . ?
C5 C1 C2 108.6(8) . . ?
C5 C1 Gd1 73.9(4) . . ?
C2 C1 Gd1 75.3(4) . . ?
C3 C2 C1 107.2(7) . . ?
C3 C2 Gd1 73.3(4) . . ?
C1 C2 Gd1 74.9(3) . . ?
C2 C3 C4 106.0(8) . . ?
C2 C3 Gd1 77.0(4) . . ?
C4 C3 Gd1 75.3(4) . . ?
C5 C4 C3 108.7(8) . . ?
C5 C4 Gd1 75.0(4) . . ?
C3 C4 Gd1 74.4(4) . . ?
C1 C5 C4 109.3(8) . . ?
C1 C5 Gd1 77.4(4) . . ?
C4 C5 Gd1 76.0(4) . . ?
C10 C6 C7 110.6(8) . . ?
C10 C6 Gd1 74.8(4) . . ?
C7 C6 Gd1 76.6(4) . . ?
C6 C7 C8 108.9(7) . . ?
C6 C7 Gd1 74.8(4) . . ?
C8 C7 Gd1 74.7(4) . . ?
C7 C8 C9 105.7(7) . . ?
C7 C8 Gd1 76.0(4) . . ?
C9 C8 Gd1 73.9(4) . . ?
C10 C9 C8 106.1(7) . . ?
C10 C9 Gd1 74.7(4) . . ?
C8 C9 Gd1 75.2(3) . . ?
C6 C10 C9 108.6(8) . . ?
C6 C10 Gd1 76.6(4) . . ?
C9 C10 Gd1 75.6(4) . . ?
N1 C11 O1 113.1(4) . . ?
N1 C11 N2 129.8(4) . . ?
O1 C11 N2 116.9(4) . . ?
N1 C11 Gd1 57.3(2) . . ?
O1 C11 Gd1 55.9(2) . . ?
N2 C11 Gd1 170.5(3) . . ?
N2 C12 N3 124.6(5) . . ?
N2 C12 N4 118.9(5) . . ?
N3 C12 N4 116.3(5) . . ?
C22 C17 C18 118.7(5) . . ?
C22 C17 N1 121.9(5) . . ?
C18 C17 N1 119.3(5) . . ?
C17 C18 C19 119.6(6) . . ?
C20 C19 C18 120.7(6) . . ?
C19 C20 C21 119.8(6) . . ?
C22 C21 C20 120.2(6) . . ?
C21 C22 C17 121.1(6) . . ?
C23 O2 C26 90.9(14) . . ?
C24 C23 O2 100.0(12) . . ?
C23 C24 C25 95.4(16) . . ?
C26 C25 C24 74.9(17) . . ?
C25 C26 O2 88.5(13) . . ?
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 2.315(3) 2_656 ?
Gd1 O1 2.427(3) . ?
Gd1 N1 2.459(4) . ?
Gd1 C10 2.670(7) . ?
Gd1 C9 2.681(6) . ?
Gd1 C5 2.682(6) . ?
Gd1 C3 2.683(7) . ?
Gd1 C6 2.692(7) . ?
Gd1 C8 2.697(6) . ?
Gd1 C4 2.695(7) . ?
Gd1 C7 2.714(6) . ?
Gd1 C1 2.725(6) . ?
N1 C11 1.306(6) . ?
N1 C17 1.420(6) . ?
N2 C12 1.305(6) . ?
N2 C11 1.359(6) . ?
N3 C12 1.359(7) . ?
N3 C15 1.442(8) . ?
N3 C16 1.474(8) . ?
N4 C12 1.371(7) . ?
N4 C13 1.446(7) . ?
N4 C14 1.461(8) . ?
O1 C11 1.318(5) . ?
O1 Gd1 2.315(3) 2_656 ?
C1 C5 1.338(11) . ?
C1 C2 1.399(11) . ?
C2 C3 1.387(13) . ?
C3 C4 1.407(13) . ?
C4 C5 1.345(13) . ?
C6 C10 1.324(13) . ?
C6 C7 1.334(12) . ?
C7 C8 1.368(11) . ?
C8 C9 1.433(12) . ?
C9 C10 1.374(13) . ?
C17 C22 1.378(7) . ?
C17 C18 1.382(7) . ?
C18 C19 1.400(8) . ?
C19 C20 1.353(10) . ?
C20 C21 1.373(10) . ?
C21 C22 1.369(8) . ?
O2 C23 1.489(15) . ?
O2 C26 1.577(17) . ?
C23 C24 1.486(15) . ?
C24 C25 1.495(19) . ?
C25 C26 1.481(18) . ?
