#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:30:38 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178902 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/31/4113145.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_4113145
loop_
_publ_author_name
'William J. Evans'
'David S. Lee'
'Daniel B. Rego'
'Jeremy M. Perotti'
'Stosh A. Kozimor'
'Ericka K. Moore'
'Joseph W. Ziller'
_publ_section_title
;
 Expanding Dinitrogen Reduction Chemistry to Trivalent Lanthanides via the
 LnZ3/Alkali Metal Reduction System: Evaluation of the Generality of
 Forming Ln2(μ-η2:η2-N2) Complexes via LnZ3/K
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14574
_journal_page_last               14582
_journal_paper_doi               10.1021/ja046047s
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C32 H88 Gd2 N6 O2 Si8'
_chemical_formula_weight         1128.30
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXTL
_cell_angle_alpha                90.00
_cell_angle_beta                 112.585(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.8414(18)
_cell_length_b                   23.469(4)
_cell_length_c                   11.5946(19)
_cell_measurement_temperature    163(2)
_cell_volume                     2723.9(8)
_computing_cell_refinement       'Bruker SMART/SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      163(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_sigmaI/netI    0.0251
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            27741
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         2.09
_diffrn_standards_decay_%        '< 1.0'
_diffrn_standards_interval_count 'initial 50 frames recollected'
_diffrn_standards_number         '50 frames'
_exptl_absorpt_coefficient_mu    2.620
_exptl_absorpt_correction_T_max  0.5964
_exptl_absorpt_correction_T_min  0.4058
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            pale
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_density_meas      ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1156
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.871
_refine_diff_density_min         -0.588
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         6560
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0312
_refine_ls_R_factor_gt           0.0223
_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)+(0.0155P)²+3.1251P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0470
_refine_ls_wR_factor_ref         0.0500
_reflns_number_gt                5624
_reflns_number_total             6560
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja046047ssi20040813_055805.cif
_cod_data_source_block           dbr5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'n/a' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4113145
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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 0.053708(11) 0.090394(5) 0.974093(10) 0.01603(4) Uani 1 1 d . . .
Si1 Si -0.00599(7) 0.17465(3) 1.18605(6) 0.02049(13) Uani 1 1 d . . .
Si2 Si 0.26186(7) 0.11491(3) 1.28001(6) 0.02541(15) Uani 1 1 d . . .
Si3 Si 0.24340(7) 0.16966(3) 0.86528(6) 0.02258(14) Uani 1 1 d . . .
Si4 Si 0.24874(7) 0.04577(3) 0.80361(6) 0.02052(13) Uani 1 1 d . . .
O1 O -0.13970(17) 0.11016(8) 0.78285(16) 0.0262(4) Uani 1 1 d . . .
N1 N 0.1104(2) 0.13084(8) 1.16625(17) 0.0197(4) Uani 1 1 d . A .
N2 N 0.19904(19) 0.10042(8) 0.87439(17) 0.0174(4) Uani 1 1 d . A .
N3 N 0.0623(2) -0.00563(9) 1.0263(2) 0.0269(5) Uani 1 1 d . . .
C1 C -0.0569(3) 0.15284(13) 1.3170(3) 0.0340(6) Uani 1 1 d . . .
H1A H -0.0855 0.1129 1.3061 0.051 Uiso 1 1 calc R . .
H1B H -0.1308 0.1769 1.3166 0.051 Uiso 1 1 calc R . .
H1C H 0.0192 0.1573 1.3968 0.051 Uiso 1 1 calc R . .
C2 C 0.0478(3) 0.25125(11) 1.2117(3) 0.0303(6) Uani 1 1 d . . .
H2A H 0.0749 0.2639 1.1444 0.045 Uiso 1 1 calc R . .
H2B H 0.1233 0.2551 1.2921 0.045 Uiso 1 1 calc R . .
H2C H -0.0267 0.2748 1.2121 0.045 Uiso 1 1 calc R . .
C3 C -0.1603(3) 0.17169(12) 1.0384(2) 0.0283(6) Uani 1 1 d . . .
H3A H -0.1915 0.1322 1.0217 0.042 Uiso 1 1 calc R . .
H3B H -0.1395 0.1860 0.9685 0.042 Uiso 1 1 calc R . .
H3C H -0.2303 0.1953 1.0479 0.042 Uiso 1 1 calc R . .
C4 C 0.3678(6) 0.1827(3) 1.3350(7) 0.0385(19) Uiso 0.543(14) 1 d P A 1
H4A H 0.3241 0.2087 1.3737 0.058 Uiso 0.543(14) 1 calc PR A 1
H4B H 0.3769 0.2016 1.2631 0.058 Uiso 0.543(14) 1 calc PR A 1
H4C H 0.4566 0.1726 1.3960 0.058 Uiso 0.543(14) 1 calc PR A 1
C5 C 0.2364(7) 0.0577(4) 1.3924(6) 0.037(2) Uiso 0.530(18) 1 d P A 1
H5A H 0.1812 0.0738 1.4343 0.055 Uiso 0.530(18) 1 calc PR A 1
H5B H 0.3235 0.0466 1.4551 0.055 Uiso 0.530(18) 1 calc PR A 1
H5C H 0.1919 0.0241 1.3440 0.055 Uiso 0.530(18) 1 calc PR A 1
C4B C 0.3457(8) 0.1742(3) 1.3855(8) 0.040(2) Uiso 0.457(14) 1 d P A 2
H4B1 H 0.3653 0.2047 1.3374 0.060 Uiso 0.457(14) 1 calc PR A 2
H4B2 H 0.4293 0.1605 1.4497 0.060 Uiso 0.457(14) 1 calc PR A 2
H4B3 H 0.2872 0.1888 1.4253 0.060 Uiso 0.457(14) 1 calc PR A 2
C5B C 0.2599(8) 0.0812(4) 1.4164(7) 0.034(2) Uiso 0.470(18) 1 d P A 2
H5B1 H 0.2039 0.1032 1.4493 0.051 Uiso 0.470(18) 1 calc PR A 2
H5B2 H 0.3512 0.0792 1.4796 0.051 Uiso 0.470(18) 1 calc PR A 2
H5B3 H 0.2237 0.0426 1.3956 0.051 Uiso 0.470(18) 1 calc PR A 2
C6 C 0.3676(3) 0.07529(14) 1.2127(3) 0.0370(7) Uani 1 1 d . A .
H6A H 0.4541 0.0665 1.2791 0.055 Uiso 1 1 calc R . .
H6B H 0.3815 0.0988 1.1489 0.055 Uiso 1 1 calc R . .
H6C H 0.3227 0.0398 1.1747 0.055 Uiso 1 1 calc R . .
C7 C 0.4240(3) 0.18593(14) 0.9598(3) 0.0410(7) Uani 1 1 d . A .
H7A H 0.4476 0.1723 1.0456 0.061 Uiso 1 1 calc R . .
H7B H 0.4384 0.2272 0.9606 0.061 Uiso 1 1 calc R . .
H7C H 0.4801 0.1668 0.9226 0.061 Uiso 1 1 calc R . .
C8 C 0.1452(4) 0.21673(12) 0.9311(3) 0.0431(8) Uani 1 1 d . A .
H8A H 0.1622 0.2051 1.0170 0.065 Uiso 1 1 calc R . .
H8B H 0.0497 0.2131 0.8799 0.065 Uiso 1 1 calc R . .
H8C H 0.1729 0.2565 0.9305 0.065 Uiso 1 1 calc R . .
C9 C 0.2020(3) 0.19631(12) 0.7015(2) 0.0317(6) Uani 1 1 d . A .
H9A H 0.1080 0.1883 0.6507 0.048 Uiso 1 1 calc R . .
H9B H 0.2589 0.1770 0.6653 0.048 Uiso 1 1 calc R . .
H9C H 0.2177 0.2375 0.7034 0.048 Uiso 1 1 calc R . .
C10 C 0.1091(3) 0.02441(15) 0.6557(3) 0.0463(8) Uani 1 1 d . A .
H10A H 0.0814 0.0573 0.5994 0.069 Uiso 1 1 calc R . .
H10B H 0.0334 0.0110 0.6747 0.069 Uiso 1 1 calc R . .
H10C H 0.1394 -0.0062 0.6154 0.069 Uiso 1 1 calc R . .
C11 C 0.3971(3) 0.06259(14) 0.7646(3) 0.0378(7) Uani 1 1 d . A .
H11A H 0.3783 0.0965 0.7114 0.057 Uiso 1 1 calc R . .
H11B H 0.4158 0.0303 0.7203 0.057 Uiso 1 1 calc R . .
H11C H 0.4748 0.0698 0.8418 0.057 Uiso 1 1 calc R . .
C12 C 0.2961(4) -0.01898(13) 0.9050(3) 0.0451(8) Uani 1 1 d . A .
H12A H 0.2219 -0.0299 0.9288 0.068 Uiso 1 1 calc R . .
H12B H 0.3752 -0.0106 0.9804 0.068 Uiso 1 1 calc R . .
H12C H 0.3162 -0.0503 0.8591 0.068 Uiso 1 1 calc R . .
C13 C -0.1399(3) 0.13864(13) 0.6719(3) 0.0340(6) Uani 1 1 d . A .
H13A H -0.0522 0.1346 0.6649 0.041 Uiso 1 1 calc R . .
H13B H -0.1602 0.1797 0.6737 0.041 Uiso 1 1 calc R . .
C14 C -0.2483(3) 0.10910(15) 0.5646(3) 0.0414(7) Uani 1 1 d . . .
H14A H -0.2908 0.1357 0.4942 0.050 Uiso 1 1 calc R A .
H14B H -0.2117 0.0762 0.5345 0.050 Uiso 1 1 calc R . .
C15 C -0.3466(3) 0.08972(18) 0.6192(3) 0.0525(9) Uani 1 1 d . A .
H15A H -0.4264 0.1147 0.5904 0.063 Uiso 1 1 calc R . .
H15B H -0.3756 0.0501 0.5931 0.063 Uiso 1 1 calc R . .
C16 C -0.2776(3) 0.09299(15) 0.7563(3) 0.0397(7) Uani 1 1 d . A .
H16A H -0.3220 0.1213 0.7908 0.048 Uiso 1 1 calc R . .
H16B H -0.2796 0.0555 0.7945 0.048 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'
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'
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
N1 Gd1 N2 118.03(7) . .
N1 Gd1 N3 100.39(8) . .
N2 Gd1 N3 105.29(7) . .
N1 Gd1 N3 107.31(8) . 3_557
N2 Gd1 N3 123.73(7) . 3_557
N3 Gd1 N3 31.70(10) . 3_557
N1 Gd1 O1 128.63(7) . .
N2 Gd1 O1 92.25(6) . .
N3 Gd1 O1 110.81(7) . .
N3 Gd1 O1 83.50(7) 3_557 .
N1 Gd1 Si3 99.35(5) . .
N2 Gd1 Si3 27.92(5) . .
N3 Gd1 Si3 131.72(6) . .
N3 Gd1 Si3 150.67(6) 3_557 .
O1 Gd1 Si3 89.41(4) . .
N1 Gd1 Si1 26.73(5) . .
N2 Gd1 Si1 131.40(5) . .
N3 Gd1 Si1 111.99(6) . .
N3 Gd1 Si1 104.06(6) 3_557 .
O1 Gd1 Si1 102.14(5) . .
Si3 Gd1 Si1 105.26(2) . .
N1 Gd1 Si2 25.72(5) . .
N2 Gd1 Si2 101.33(5) . .
N3 Gd1 Si2 87.07(6) . .
N3 Gd1 Si2 106.37(6) 3_557 .
O1 Gd1 Si2 153.97(5) . .
Si3 Gd1 Si2 92.34(2) . .
Si1 Gd1 Si2 52.441(19) . .
N1 Si1 C1 113.98(12) . .
N1 Si1 C2 113.35(12) . .
C1 Si1 C2 107.63(13) . .
N1 Si1 C3 107.45(11) . .
C1 Si1 C3 106.97(13) . .
C2 Si1 C3 107.06(12) . .
N1 Si1 Gd1 36.80(7) . .
C1 Si1 Gd1 128.51(9) . .
C2 Si1 Gd1 122.47(9) . .
C3 Si1 Gd1 70.76(8) . .
N1 Si2 C5B 116.7(3) . .
N1 Si2 C4B 115.5(2) . .
C5B Si2 C4B 85.2(5) . .
N1 Si2 C6 110.45(12) . .
C5B Si2 C6 111.7(3) . .
C4B Si2 C6 115.3(3) . .
N1 Si2 C4 110.5(2) . .
C5B Si2 C4 106.5(4) . .
C4B Si2 C4 22.6(2) . .
C6 Si2 C4 99.6(2) . .
N1 Si2 C5 108.9(2) . .
C5B Si2 C5 18.4(2) . .
C4B Si2 C5 103.6(4) . .
C6 Si2 C5 101.7(2) . .
C4 Si2 C5 124.4(4) . .
N1 Si2 Gd1 35.41(7) . .
C5B Si2 Gd1 128.0(3) . .
C4B Si2 Gd1 140.4(3) . .
C6 Si2 Gd1 75.55(10) . .
C4 Si2 Gd1 123.5(2) . .
C5 Si2 Gd1 111.5(3) . .
N2 Si3 C7 114.32(12) . .
N2 Si3 C9 114.49(11) . .
C7 Si3 C9 108.19(13) . .
N2 Si3 C8 108.42(11) . .
C7 Si3 C8 105.55(16) . .
C9 Si3 C8 105.10(14) . .
N2 Si3 Gd1 38.98(7) . .
C7 Si3 Gd1 122.99(9) . .
C9 Si3 Gd1 128.32(9) . .
C8 Si3 Gd1 69.54(9) . .
N2 Si4 C10 110.29(13) . .
N2 Si4 C12 111.57(11) . .
C10 Si4 C12 106.84(17) . .
N2 Si4 C11 114.46(12) . .
C10 Si4 C11 107.65(15) . .
C12 Si4 C11 105.62(15) . .
C13 O1 C16 106.7(2) . .
C13 O1 Gd1 127.04(15) . .
C16 O1 Gd1 126.23(15) . .
Si2 N1 Si1 124.64(12) . .
Si2 N1 Gd1 118.88(10) . .
Si1 N1 Gd1 116.47(10) . .
Si3 N2 Si4 122.22(11) . .
Si3 N2 Gd1 113.09(10) . .
Si4 N2 Gd1 124.47(10) . .
N3 N3 Gd1 75.28(19) 3_557 .
N3 N3 Gd1 73.01(18) 3_557 3_557
Gd1 N3 Gd1 148.30(10) . 3_557
O1 C13 C14 104.8(2) . .
C15 C14 C13 104.1(2) . .
C16 C15 C14 106.8(2) . .
O1 C16 C15 107.2(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Gd1 N1 2.2782(19) .
Gd1 N2 2.2964(19) .
Gd1 N3 2.326(2) .
Gd1 N3 2.353(2) 3_557
Gd1 O1 2.4408(17) .
Gd1 Si3 3.3578(7) .
Gd1 Si1 3.4044(7) .
Gd1 Si2 3.4434(8) .
Si1 N1 1.710(2) .
Si1 C1 1.875(3) .
Si1 C2 1.878(3) .
Si1 C3 1.880(3) .
Si2 N1 1.706(2) .
Si2 C5B 1.775(7) .
Si2 C4B 1.844(7) .
Si2 C6 1.864(3) .
Si2 C4 1.923(6) .
Si2 C5 1.963(7) .
Si3 N2 1.709(2) .
Si3 C7 1.879(3) .
Si3 C9 1.882(3) .
Si3 C8 1.887(3) .
Si4 N2 1.717(2) .
Si4 C10 1.868(3) .
Si4 C12 1.869(3) .
Si4 C11 1.872(3) .
O1 C13 1.448(3) .
O1 C16 1.463(3) .
N3 N3 1.278(4) 3_557
N3 Gd1 2.353(2) 3_557
C13 C14 1.512(4) .
C14 C15 1.504(5) .
C15 C16 1.476(4) .
