#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:34:46 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179336 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/33/4323345.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_4323345
loop_
_publ_author_name
'Syed A. A. Shah'
'Hendrik Dorn'
'Herbert W. Roesky'
'Paolo Lubini'
'Hans-Georg Schmidt'
_publ_section_title
;
 Novel Cyclopentadienyl-Free Organolanthanides: The First Examples of
 Five-Membered Amidolanthanide Heterocycles
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1102
_journal_page_last               1106
_journal_paper_doi               10.1021/ic961033b
_journal_volume                  36
_journal_year                    1997
_chemical_formula_sum            'C39 H84 Cl2 Gd2 N4 O2 Si4'
_chemical_formula_weight         1138.86
_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
_cell_angle_alpha                107.57(3)
_cell_angle_beta                 111.31(3)
_cell_angle_gamma                90.67(3)
_cell_formula_units_Z            1
_cell_length_a                   10.321(2)
_cell_length_b                   11.116(2)
_cell_length_c                   13.434(3)
_cell_measurement_temperature    120(2)
_cell_volume                     1356.0(6)
_computing_structure_refinement  'SHELXL-96 (Sheldrick, 1996)'
_computing_structure_solution    'SHELXS-96 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_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  0.0201
_diffrn_reflns_av_sigmaI/netI    0.0094
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6013
_diffrn_reflns_theta_max         25.11
_diffrn_reflns_theta_min         3.69
_exptl_absorpt_coefficient_mu    2.643
_exptl_absorpt_correction_T_max  0.8094
_exptl_absorpt_correction_T_min  0.7477
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_description       blocks
_exptl_crystal_F_000             580
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.016
_refine_diff_density_min         -1.741
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.185
_refine_ls_goodness_of_fit_obs   1.185
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         4767
_refine_ls_number_restraints     169
_refine_ls_restrained_S_all      1.170
_refine_ls_restrained_S_obs      1.169
_refine_ls_R_factor_all          0.0234
_refine_ls_R_factor_obs          0.0233
_refine_ls_shift/esd_max         0.014
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0356P)²+2.0031P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0634
_refine_ls_wR_factor_obs         0.0633
_reflns_number_observed          4760
_reflns_number_total             4767
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic961033b_1.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0356P)^2^+2.0031P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0356P)^2^+2.0031P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1356.1(5)
_cod_database_code               4323345
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Gd1 Gd -0.006342(13) -0.109800(12) -0.164390(10) 0.01503(6) Uani 1 d . .
Cl1 Cl 0.17632(7) 0.05734(7) 0.04328(6) 0.02424(16) Uani 1 d . .
N1 N -0.0497(3) -0.3194(2) -0.2274(2) 0.0206(5) Uani 1 d . .
O1 O 0.2061(2) -0.1102(2) -0.19890(18) 0.0259(5) Uani 1 d . .
Si1 Si -0.19935(9) -0.36613(8) -0.34938(7) 0.02175(18) Uani 1 d . .
C1 C 0.0275(4) -0.4021(3) -0.1646(3) 0.0270(7) Uani 1 d . .
N2 N -0.1325(3) -0.0576(2) -0.3140(2) 0.0199(5) Uani 1 d . .
Si2 Si -0.23401(9) -0.19153(8) -0.42070(7) 0.02146(18) Uani 1 d . .
C2 C 0.1227(5) -0.3149(4) -0.0461(3) 0.0409(9) Uani 1 d . .
H2A H 0.1874 -0.2550 -0.0523 0.061 Uiso 1 calc R .
H2B H 0.1766 -0.3666 -0.0022 0.061 Uiso 1 calc R .
H2C H 0.0651 -0.2674 -0.0079 0.061 Uiso 1 calc R .
C3 C 0.1181(5) -0.4772(4) -0.2223(3) 0.0424(9) Uani 1 d . .
H3A H 0.1871 -0.4179 -0.2246 0.064 Uiso 1 calc R .
H3B H 0.0583 -0.5299 -0.2996 0.064 Uiso 1 calc R .
H3C H 0.1669 -0.5320 -0.1798 0.064 Uiso 1 calc R .
C4 C -0.0730(5) -0.4936(4) -0.1519(3) 0.0413(9) Uani 1 d . .
H4A H -0.0186 -0.5423 -0.1051 0.062 Uiso 1 calc R .
H4B H -0.1327 -0.5523 -0.2268 0.062 Uiso 1 calc R .
H4C H -0.1318 -0.4449 -0.1159 0.062 Uiso 1 calc R .
C5 C -0.1917(4) -0.5078(3) -0.4674(3) 0.0385(9) Uani 1 d . .
H5A H -0.1094 -0.4912 -0.4837 0.058 Uiso 1 calc R .
H5B H -0.2770 -0.5217 -0.5355 0.058 Uiso 1 calc R .
H5C H -0.1850 -0.5838 -0.4442 0.058 Uiso 1 calc R .
C6 C -0.3641(4) -0.4087(4) -0.3292(4) 0.0388(9) Uani 1 d . .
H6A H -0.3669 -0.3456 -0.2612 0.058 Uiso 1 calc R .
H6B H -0.3640 -0.4933 -0.3208 0.058 Uiso 1 calc R .
H6C H -0.4468 -0.4094 -0.3952 0.058 Uiso 1 calc R .
C7 C -0.1897(4) -0.2396(4) -0.5511(3) 0.0376(8) Uani 1 d . .
H7A H -0.2124 -0.1749 -0.5885 0.056 Uiso 1 calc R .
H7B H -0.2446 -0.3218 -0.6033 0.056 Uiso 1 calc R .
H7C H -0.0894 -0.2468 -0.5290 0.056 Uiso 1 calc R .
C8 C -0.4278(4) -0.1810(4) -0.4758(4) 0.0413(9) Uani 1 d . .
H8A H -0.4584 -0.1540 -0.4123 0.062 Uiso 1 calc R .
H8B H -0.4792 -0.2647 -0.5276 0.062 Uiso 1 calc R .
H8C H -0.4467 -0.1189 -0.5161 0.062 Uiso 1 calc R .
C9 C -0.1348(4) 0.0750(3) -0.3138(3) 0.0271(7) Uani 1 d . .
C10 C -0.1605(5) 0.0860(4) -0.4302(3) 0.0401(9) Uani 1 d . .
H10A H -0.1562 0.1760 -0.4247 0.060 Uiso 1 calc R .
H10B H -0.2533 0.0407 -0.4841 0.060 Uiso 1 calc R .
H10C H -0.0883 0.0483 -0.4562 0.060 Uiso 1 calc R .
C11 C -0.2502(4) 0.1321(3) -0.2752(3) 0.0355(8) Uani 1 d . .
H11A H -0.2339 0.1266 -0.2002 0.053 Uiso 1 calc R .
H11B H -0.3419 0.0846 -0.3293 0.053 Uiso 1 calc R .
H11C H -0.2483 0.2216 -0.2714 0.053 Uiso 1 calc R .
C12 C 0.0078(4) 0.1518(3) -0.2308(3) 0.0390(9) Uani 1 d . .
H12A H 0.0086 0.2400 -0.2307 0.059 Uiso 1 calc R .
H12B H 0.0820 0.1141 -0.2539 0.059 Uiso 1 calc R .
H12C H 0.0240 0.1504 -0.1546 0.059 Uiso 1 calc R .
C50 C 0.1950(4) -0.1773(4) -0.3138(3) 0.0355(8) Uani 1 d U .
H50A_a H 0.1475 -0.1303 -0.3659 0.043 Uiso 1 calc R 1
H50B_a H 0.1434 -0.2643 -0.3428 0.043 Uiso 1 calc R 1
C51_a C 0.3457(16) -0.1808(15) -0.2991(10) 0.072(4) Uani 0.740(16) d PU 1
H51A_a H 0.3770 -0.2592 -0.2830 0.086 Uiso 0.740(16) calc PR 1
H51B_a H 0.3566 -0.1814 -0.3695 0.086 Uiso 0.740(16) calc PR 1
C52_a C 0.4250(6) -0.0770(9) -0.2123(6) 0.058(3) Uani 0.740(16) d PU 1
H52A_a H 0.4253 -0.0021 -0.2376 0.070 Uiso 0.740(16) calc PR 1
H52B_a H 0.5229 -0.0930 -0.1780 0.070 Uiso 0.740(16) calc PR 1
C53_a C 0.351(2) -0.0569(17) -0.1279(18) 0.051(4) Uani 0.740(16) d PU 1
H53A_a H 0.3919 -0.1020 -0.0728 0.062 Uiso 0.740(16) calc PR 1
H53B_a H 0.3584 0.0348 -0.0862 0.062 Uiso 0.740(16) calc PR 1
C51_b C 0.339(4) -0.209(3) -0.316(3) 0.039(5) Uani 0.260(16) d PU 2
H51C_b H 0.3372 -0.3013 -0.3515 0.046 Uiso 0.260(16) calc PR 2
H51D_b H 0.3709 -0.1615 -0.3568 0.046 Uiso 0.260(16) calc PR 2
C52_b C 0.4271(17) -0.164(2) -0.1921(14) 0.046(5) Uani 0.260(16) d PU 2
H52C_b H 0.4543 -0.2385 -0.1678 0.056 Uiso 0.260(16) calc PR 2
H52D_b H 0.5141 -0.1115 -0.1783 0.056 Uiso 0.260(16) calc PR 2
C53_b C 0.356(5) -0.089(5) -0.124(5) 0.047(9) Uani 0.260(16) d PU 2
H53C_b H 0.3942 0.0021 -0.0965 0.056 Uiso 0.260(16) calc PR 2
H53D_b H 0.3693 -0.1175 -0.0586 0.056 Uiso 0.260(16) calc PR 2
C80 C 0.460(2) 0.4802(16) 0.0573(15) 0.097(6) Uani 0.50 d PDU -1
H80 H 0.4114 0.4211 0.0745 0.116 Uiso 0.50 calc PR -1
C81 C 0.4991(15) 0.6022(15) 0.1267(11) 0.113(5) Uani 0.50 d PDU -1
H81 H 0.4784 0.6288 0.1928 0.136 Uiso 0.50 calc PR -1
C82 C 0.568(2) 0.6870(17) 0.1023(16) 0.112(6) Uani 0.50 d PDU -1
H82 H 0.5948 0.7729 0.1512 0.135 Uiso 0.50 calc PR -1
C83 C 0.5981(13) 0.6494(12) 0.0078(12) 0.093(4) Uani 0.50 d PDU -1
H83 H 0.6475 0.7079 -0.0093 0.111 Uiso 0.50 calc PR -1
C84 C 0.557(3) 0.5270(14) -0.0613(17) 0.092(6) Uani 0.50 d PDU -1
H84 H 0.5749 0.5002 -0.1284 0.110 Uiso 0.50 calc PR -1
C85 C 0.4893(12) 0.4421(11) -0.0364(10) 0.086(3) Uani 0.50 d PDU -1
C86 C 0.445(3) 0.302(2) -0.116(2) 0.163(11) Uani 0.50 d PDU -1
H86A H 0.3762 0.2987 -0.1902 0.244 Uiso 0.50 calc PR -1
H86B H 0.4035 0.2522 -0.0834 0.244 Uiso 0.50 calc PR -1
H86C H 0.5279 0.2655 -0.1254 0.244 Uiso 0.50 calc PR -1
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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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
N1 Gd1 N2 102.97(10) . . ?
N1 Gd1 O1 92.70(9) . . ?
N2 Gd1 O1 95.19(9) . . ?
N1 Gd1 Cl1 99.26(7) . 2 ?
N2 Gd1 Cl1 100.10(7) . 2 ?
O1 Gd1 Cl1 157.90(5) . 2 ?
N1 Gd1 Cl1 130.72(7) . . ?
N2 Gd1 Cl1 126.13(7) . . ?
O1 Gd1 Cl1 80.14(6) . . ?
Cl1 Gd1 Cl1 77.96(3) 2 . ?
N1 Gd1 Si1 30.63(7) . . ?
N2 Gd1 Si1 73.77(7) . . ?
O1 Gd1 Si1 104.23(6) . . ?
Cl1 Gd1 Si1 95.36(3) 2 . ?
Cl1 Gd1 Si1 159.62(3) . . ?
N1 Gd1 Si2 72.98(8) . . ?
N2 Gd1 Si2 30.18(7) . . ?
O1 Gd1 Si2 99.78(6) . . ?
Cl1 Gd1 Si2 101.47(3) 2 . ?
Cl1 Gd1 Si2 156.27(3) . . ?
Si1 Gd1 Si2 43.64(3) . . ?
Gd1 Cl1 Gd1 102.04(3) 2 . ?
C1 N1 Si1 126.6(2) . . ?
C1 N1 Gd1 124.14(19) . . ?
Si1 N1 Gd1 108.71(13) . . ?
C53_a O1 C50 109.5(8) . . ?
C50 O1 C53_b 107(2) . . ?
C53_a O1 Gd1 133.5(7) . . ?
C50 O1 Gd1 117.00(18) . . ?
C53_b O1 Gd1 133(2) . . ?
N1 Si1 C6 114.59(16) . . ?
N1 Si1 C5 115.35(16) . . ?
C6 Si1 C5 105.10(19) . . ?
N1 Si1 Si2 107.05(10) . . ?
C6 Si1 Si2 107.86(13) . . ?
C5 Si1 Si2 106.41(13) . . ?
N1 Si1 Gd1 40.66(9) . . ?
C6 Si1 Gd1 114.71(13) . . ?
C5 Si1 Gd1 139.54(14) . . ?
Si2 Si1 Gd1 68.62(4) . . ?
N1 C1 C3 111.1(3) . . ?
N1 C1 C2 107.2(3) . . ?
C3 C1 C2 109.0(3) . . ?
N1 C1 C4 111.4(3) . . ?
C3 C1 C4 109.9(3) . . ?
C2 C1 C4 108.2(3) . . ?
C9 N2 Si2 127.1(2) . . ?
C9 N2 Gd1 123.15(19) . . ?
Si2 N2 Gd1 109.52(13) . . ?
N2 Si2 C8 114.54(17) . . ?
N2 Si2 C7 115.13(15) . . ?
C8 Si2 C7 104.65(19) . . ?
N2 Si2 Si1 107.96(9) . . ?
C8 Si2 Si1 107.76(14) . . ?
C7 Si2 Si1 106.30(13) . . ?
N2 Si2 Gd1 40.30(8) . . ?
C8 Si2 Gd1 130.09(14) . . ?
C7 Si2 Gd1 124.71(13) . . ?
Si1 Si2 Gd1 67.74(4) . . ?
N2 C9 C10 112.7(3) . . ?
N2 C9 C11 109.7(3) . . ?
C10 C9 C11 108.9(3) . . ?
N2 C9 C12 108.4(3) . . ?
C10 C9 C12 108.0(3) . . ?
C11 C9 C12 109.2(3) . . ?
O1 C50 C51_a 102.3(5) . . ?
O1 C50 C51_b 111.3(12) . . ?
C52_a C51_a C50 109.1(9) . . ?
C51_a C52_a C53_a 103.1(10) . . ?
O1 C53_a C52_a 104.0(12) . . ?
C52_b C51_b C50 100(2) . . ?
C53_b C52_b C51_b 113(3) . . ?
C52_b C53_b O1 106(3) . . ?
C85 C80 C81 120.0(10) . . ?
C80 C81 C82 120.2(10) . . ?
C81 C82 C83 120.2(10) . . ?
C84 C83 C82 118.6(9) . . ?
C85 C84 C83 121.2(10) . . ?
C80 C85 C84 119.7(10) . . ?
C80 C85 C86 120.2(9) . . ?
C84 C85 C86 120.1(9) . . ?
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 N1 2.203(3) . ?
Gd1 N2 2.211(2) . ?
Gd1 O1 2.400(2) . ?
Gd1 Cl1 2.7550(10) 2 ?
Gd1 Cl1 2.7849(17) . ?
Gd1 Si1 3.2027(19) . ?
Gd1 Si2 3.2225(17) . ?
Cl1 Gd1 2.7550(10) 2 ?
N1 C1 1.479(4) . ?
N1 Si1 1.723(3) . ?
O1 C53_a 1.447(19) . ?
O1 C50 1.458(4) . ?
O1 C53_b 1.48(5) . ?
Si1 C6 1.893(4) . ?
Si1 C5 1.894(4) . ?
Si1 Si2 2.3881(13) . ?
C1 C3 1.525(5) . ?
C1 C2 1.533(5) . ?
C1 C4 1.532(5) . ?
N2 C9 1.473(4) . ?
N2 Si2 1.719(3) . ?
Si2 C8 1.883(4) . ?
Si2 C7 1.894(4) . ?
C9 C10 1.532(5) . ?
C9 C11 1.536(5) . ?
C9 C12 1.530(5) . ?
C50 C51_a 1.498(16) . ?
C50 C51_b 1.54(4) . ?
C51_a C52_a 1.354(13) . ?
C52_a C53_a 1.551(19) . ?
C51_b C52_b 1.50(4) . ?
C52_b C53_b 1.44(6) . ?
C80 C85 1.347(12) . ?
C80 C81 1.351(13) . ?
C81 C82 1.355(14) . ?
C82 C83 1.363(13) . ?
C83 C84 1.353(12) . ?
C84 C85 1.351(12) . ?
C85 C86 1.55(3) . ?
