#------------------------------------------------------------------------------
#$Date: 2016-10-08 01:06:07 +0300 (Sat, 08 Oct 2016) $
#$Revision: 187077 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/04/7040494.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_7040494
loop_
_publ_author_name
'Levin, Jessica R.'
'Cheisson, Thibault'
'Carroll, Patrick J.'
'Schelter, Eric J.'
_publ_section_title
;
 Accessing relatively electron poor cerium(iv) hydrazido complexes by
 lithium cation promoted ligand reduction.
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15249
_journal_page_last               15258
_journal_paper_doi               10.1039/c6dt03154d
_journal_volume                  45
_journal_year                    2016
_chemical_formula_sum            'C64 H80 Ce Li4 N8 O4'
_chemical_formula_weight         1193.24
_space_group_IT_number           70
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      70
_symmetry_space_group_name_Hall  '-F 2uv 2vw'
_symmetry_space_group_name_H-M   'F d d d :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-08-06 deposited with the CCDC.
2016-08-24 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.362(2)
_cell_length_b                   41.867(8)
_cell_length_c                   26.271(5)
_cell_measurement_temperature    143(1)
_cell_volume                     12497(4)
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      143(1)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'CCD Area Detector'
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       'phi and 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  0.0212
_diffrn_reflns_av_sigmaI/netI    0.0056
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_k_min       -54
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            93774
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.44
_exptl_absorpt_coefficient_mu    0.780
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6730
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2007)'
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4976
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.315
_refine_diff_density_min         -0.187
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     189
_refine_ls_number_reflns         3580
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.0171
_refine_ls_R_factor_gt           0.0164
_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)+(0.0162P)²+22.8592P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0421
_refine_ls_wR_factor_ref         0.0430
_reflns_number_gt                3504
_reflns_number_total             3580
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6dt03154d2.cif
_cod_data_source_block           CMPD1
_cod_depositor_comments
'Adding full bibliography for 7040494--7040497.cif.'
_cod_original_sg_symbol_H-M      'F d d d '
_cod_database_code               7040494
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/4, z+1/4'
'x+1/4, -y, z+1/4'
'-x+1/4, -y+3/4, z+1/2'
'x, y+1/2, z+1/2'
'-x, y+3/4, z+3/4'
'x+1/4, -y+1/2, z+3/4'
'-x+1/4, -y+5/4, z+1'
'x+1/2, y, z+1/2'
'-x+1/2, y+1/4, z+3/4'
'x+3/4, -y, z+3/4'
'-x+3/4, -y+3/4, z+1'
'x+1/2, y+1/2, z'
'-x+1/2, y+3/4, z+1/4'
'x+3/4, -y+1/2, z+1/4'
'-x+3/4, -y+5/4, z+1/2'
'-x, -y, -z'
'x, -y-1/4, -z-1/4'
'-x-1/4, y, -z-1/4'
'x-1/4, y-3/4, -z-1/2'
'-x, -y+1/2, -z+1/2'
'x, -y+1/4, -z+1/4'
'-x-1/4, y+1/2, -z+1/4'
'x-1/4, y-1/4, -z'
'-x+1/2, -y, -z+1/2'
'x+1/2, -y-1/4, -z+1/4'
'-x+1/4, y, -z+1/4'
'x+1/4, y-3/4, -z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/4, -z-1/4'
'-x+1/4, y+1/2, -z-1/4'
'x+1/4, y-1/4, -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
Ce1 Ce 0.6250 0.1250 0.6250 0.01812(4) Uani 1 4 d S
O1 O 0.6250 0.1250 0.42772(4) 0.0264(2) Uani 1 2 d S
O2 O 0.6250 0.00287(3) 0.6250 0.0298(3) Uani 1 2 d S
N1 N 0.65260(8) 0.09006(2) 0.55035(3) 0.01970(18) Uani 1 1 d .
N2 N 0.54758(8) 0.08063(2) 0.57846(3) 0.02011(18) Uani 1 1 d .
C1 C 0.71784(10) 0.06515(3) 0.52963(4) 0.0207(2) Uani 1 1 d .
C2 C 0.67031(11) 0.03486(3) 0.51823(4) 0.0237(2) Uani 1 1 d .
H2 H 0.5921 0.0305 0.5260 0.031 Uiso 1 1 calc R
C3 C 0.73935(13) 0.01138(3) 0.49544(5) 0.0314(3) Uani 1 1 d .
H3 H 0.7068 -0.0086 0.4887 0.042 Uiso 1 1 calc R
C4 C 0.85578(13) 0.01726(3) 0.48269(5) 0.0375(3) Uani 1 1 d .
H4 H 0.9011 0.0015 0.4672 0.050 Uiso 1 1 calc R
C5 C 0.90364(12) 0.04703(3) 0.49347(5) 0.0352(3) Uani 1 1 d .
H5 H 0.9817 0.0511 0.4851 0.047 Uiso 1 1 calc R
C6 C 0.83707(11) 0.07073(3) 0.51654(5) 0.0271(2) Uani 1 1 d .
H6 H 0.8710 0.0905 0.5235 0.036 Uiso 1 1 calc R
C7 C 0.44143(10) 0.08373(2) 0.55258(4) 0.0209(2) Uani 1 1 d .
C8 C 0.33652(12) 0.08626(3) 0.58103(5) 0.0319(3) Uani 1 1 d .
H8 H 0.3399 0.0858 0.6164 0.042 Uiso 1 1 calc R
C9 C 0.22837(12) 0.08943(4) 0.55696(6) 0.0431(3) Uani 1 1 d .
H9 H 0.1603 0.0913 0.5764 0.057 Uiso 1 1 calc R
C10 C 0.22040(12) 0.08990(4) 0.50413(6) 0.0410(3) Uani 1 1 d .
H10 H 0.1479 0.0923 0.4882 0.054 Uiso 1 1 calc R
C11 C 0.32212(12) 0.08669(3) 0.47582(5) 0.0310(3) Uani 1 1 d .
H11 H 0.3174 0.0866 0.4405 0.041 Uiso 1 1 calc R
C12 C 0.43183(10) 0.08360(3) 0.49913(4) 0.0230(2) Uani 1 1 d .
H12 H 0.4991 0.0814 0.4792 0.031 Uiso 1 1 calc R
C13 C 0.72039(11) 0.11197(3) 0.39828(5) 0.0312(3) Uani 1 1 d .
H13A H 0.7926 0.1134 0.4178 0.042 Uiso 1 1 calc R
H13B H 0.7303 0.1245 0.3676 0.042 Uiso 1 1 calc R
C14 C 0.69887(13) 0.07759(3) 0.38397(5) 0.0358(3) Uani 1 1 d .
H14A H 0.6927 0.0649 0.4143 0.054 Uiso 1 1 calc R
H14B H 0.7632 0.0700 0.3636 0.054 Uiso 1 1 calc R
H14C H 0.6270 0.0760 0.3649 0.054 Uiso 1 1 calc R
C15 C 0.73011(14) -0.01593(3) 0.62671(6) 0.0409(3) Uani 1 1 d .
H15A H 0.7332 -0.0299 0.5973 0.054 Uiso 1 1 calc R
H15B H 0.7298 -0.0291 0.6570 0.054 Uiso 1 1 calc R
C16 C 0.83614(14) 0.00545(3) 0.62715(6) 0.0379(3) Uani 1 1 d .
H16A H 0.8376 0.0180 0.5965 0.057 Uiso 1 1 calc R
H16B H 0.9062 -0.0073 0.6291 0.057 Uiso 1 1 calc R
H16C H 0.8324 0.0194 0.6561 0.057 Uiso 1 1 calc R
Li1 Li 0.6250 0.1250 0.50076(11) 0.0296(6) Uani 1 2 d S
Li2 Li 0.6250 0.04856(7) 0.6250 0.0316(7) Uani 1 2 d S
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'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ce Ce -0.2486 2.6331 '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
N2 Ce1 N2 78.07(5) . 27_656
N2 Ce1 N2 118.51(4) . 8_644
N2 Ce1 N2 136.84(5) 27_656 8_644
N2 Ce1 N2 136.84(5) . 22_556
N2 Ce1 N2 118.51(4) 27_656 22_556
N2 Ce1 N2 78.07(5) 8_644 22_556
N2 Ce1 N1 34.88(3) . .
N2 Ce1 N1 84.21(3) 27_656 .
N2 Ce1 N1 90.43(3) 8_644 .
N2 Ce1 N1 156.04(3) 22_556 .
N2 Ce1 N1 84.21(3) . 27_656
N2 Ce1 N1 34.88(3) 27_656 27_656
N2 Ce1 N1 156.04(3) 8_644 27_656
N2 Ce1 N1 90.43(3) 22_556 27_656
N1 Ce1 N1 107.26(4) . 27_656
N2 Ce1 N1 90.43(3) . 8_644
N2 Ce1 N1 156.04(3) 27_656 8_644
N2 Ce1 N1 34.88(3) 8_644 8_644
N2 Ce1 N1 84.21(3) 22_556 8_644
N1 Ce1 N1 74.67(4) . 8_644
N1 Ce1 N1 165.39(4) 27_656 8_644
N2 Ce1 N1 156.04(3) . 22_556
N2 Ce1 N1 90.43(3) 27_656 22_556
N2 Ce1 N1 84.21(3) 8_644 22_556
N2 Ce1 N1 34.88(3) 22_556 22_556
N1 Ce1 N1 165.39(4) . 22_556
N1 Ce1 N1 74.67(4) 27_656 22_556
N1 Ce1 N1 107.26(4) 8_644 22_556
N2 Ce1 Li2 39.03(2) . .
N2 Ce1 Li2 39.03(2) 27_656 .
N2 Ce1 Li2 140.97(2) 8_644 .
N2 Ce1 Li2 140.97(2) 22_556 .
N1 Ce1 Li2 53.63(2) . .
N1 Ce1 Li2 53.63(2) 27_656 .
N1 Ce1 Li2 126.37(2) 8_644 .
N1 Ce1 Li2 126.37(2) 22_556 .
N2 Ce1 Li2 140.97(2) . 22_556
N2 Ce1 Li2 140.97(2) 27_656 22_556
N2 Ce1 Li2 39.03(2) 8_644 22_556
N2 Ce1 Li2 39.03(2) 22_556 22_556
N1 Ce1 Li2 126.37(2) . 22_556
N1 Ce1 Li2 126.37(2) 27_656 22_556
N1 Ce1 Li2 53.63(2) 8_644 22_556
N1 Ce1 Li2 53.63(2) 22_556 22_556
Li2 Ce1 Li2 180.0 . 22_556
N2 Ce1 Li1 59.26(2) . .
N2 Ce1 Li1 120.74(2) 27_656 .
N2 Ce1 Li1 59.26(2) 8_644 .
N2 Ce1 Li1 120.74(2) 22_556 .
N1 Ce1 Li1 37.34(2) . .
N1 Ce1 Li1 142.66(2) 27_656 .
N1 Ce1 Li1 37.34(2) 8_644 .
N1 Ce1 Li1 142.66(2) 22_556 .
Li2 Ce1 Li1 90.0 . .
Li2 Ce1 Li1 90.0 22_556 .
N2 Ce1 Li1 120.74(2) . 22_556
N2 Ce1 Li1 59.26(2) 27_656 22_556
N2 Ce1 Li1 120.74(2) 8_644 22_556
N2 Ce1 Li1 59.26(2) 22_556 22_556
N1 Ce1 Li1 142.66(2) . 22_556
N1 Ce1 Li1 37.34(2) 27_656 22_556
N1 Ce1 Li1 142.66(2) 8_644 22_556
N1 Ce1 Li1 37.34(2) 22_556 22_556
Li2 Ce1 Li1 90.0 . 22_556
Li2 Ce1 Li1 90.0 22_556 22_556
Li1 Ce1 Li1 180.0 . 22_556
C13 O1 C13 114.96(14) 8_644 .
C13 O1 Li1 122.52(7) 8_644 .
C13 O1 Li1 122.52(7) . .
C15 O2 C15 113.25(14) 27_656 .
C15 O2 Li2 123.37(7) 27_656 .
C15 O2 Li2 123.37(7) . .
C1 N1 N2 115.56(9) . .
C1 N1 Li1 112.34(9) . .
N2 N1 Li1 113.77(7) . .
C1 N1 Ce1 145.47(7) . .
N2 N1 Ce1 69.75(5) . .
Li1 N1 Ce1 93.71(7) . .
C1 N1 Li2 81.98(7) . .
N2 N1 Li2 49.30(5) . .
Li1 N1 Li2 162.71(6) . .
Ce1 N1 Li2 77.55(6) . .
C7 N2 N1 115.91(8) . .
C7 N2 Li2 137.44(9) . .
N1 N2 Li2 97.49(6) . .
C7 N2 Ce1 119.77(7) . .
N1 N2 Ce1 75.37(5) . .
Li2 N2 Ce1 92.68(7) . .
N1 C1 C2 123.60(10) . .
N1 C1 C6 118.76(10) . .
C2 C1 C6 117.55(10) . .
C3 C2 C1 120.67(12) . .
C4 C3 C2 121.05(12) . .
C3 C4 C5 118.92(12) . .
C6 C5 C4 121.16(13) . .
C5 C6 C1 120.64(12) . .
N2 C7 C12 123.66(10) . .
N2 C7 C8 118.73(10) . .
C12 C7 C8 117.58(11) . .
C9 C8 C7 120.91(12) . .
C8 C9 C10 120.89(13) . .
C11 C10 C9 118.79(12) . .
C10 C11 C12 121.36(12) . .
C11 C12 C7 120.44(11) . .
O1 C13 C14 111.94(10) . .
O2 C15 C16 110.00(11) . .
O1 Li1 N1 131.05(7) . .
O1 Li1 N1 131.05(7) . 8_644
N1 Li1 N1 97.90(14) . 8_644
O1 Li1 Ce1 180.0 . .
N1 Li1 Ce1 48.95(7) . .
N1 Li1 Ce1 48.95(7) 8_644 .
O2 Li2 N2 131.71(7) . .
O2 Li2 N2 131.71(7) . 27_656
N2 Li2 N2 96.57(14) . 27_656
O2 Li2 N1 131.18(5) . .
N2 Li2 N1 33.21(4) . .
N2 Li2 N1 87.73(10) 27_656 .
O2 Li2 N1 131.18(5) . 27_656
N2 Li2 N1 87.73(10) . 27_656
N2 Li2 N1 33.21(4) 27_656 27_656
N1 Li2 N1 97.64(10) . 27_656
O2 Li2 Ce1 180.0 . .
N2 Li2 Ce1 48.29(7) . .
N2 Li2 Ce1 48.29(7) 27_656 .
N1 Li2 Ce1 48.82(5) . .
N1 Li2 Ce1 48.82(5) 27_656 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ce1 N2 2.3915(10) .
Ce1 N2 2.3915(9) 27_656
Ce1 N2 2.3915(10) 8_644
Ce1 N2 2.3915(9) 22_556
Ce1 N1 2.4665(10) .
Ce1 N1 2.4665(10) 27_656
Ce1 N1 2.4665(10) 8_644
Ce1 N1 2.4665(10) 22_556
Ce1 Li2 3.200(3) .
Ce1 Li2 3.200(3) 22_556
Ce1 Li1 3.264(3) .
Ce1 Li1 3.264(3) 22_556
O1 C13 1.4390(14) 8_644
O1 C13 1.4390(14) .
O1 Li1 1.919(3) .
O2 C15 1.4311(16) 27_656
O2 C15 1.4311(16) .
O2 Li2 1.913(3) .
N1 C1 1.3905(14) .
N1 N2 1.4578(13) .
N1 Li1 1.984(2) .
N1 Li2 2.639(2) .
N2 C7 1.3906(14) .
N2 Li2 2.018(2) .
C1 C2 1.4106(16) .
C1 C6 1.4171(17) .
C2 C3 1.3928(16) .
C3 C4 1.387(2) .
C4 C5 1.389(2) .
C5 C6 1.3869(18) .
C7 C12 1.4085(16) .
C7 C8 1.4108(17) .
C8 C9 1.3884(19) .
C9 C10 1.391(2) .
C10 C11 1.381(2) .
C11 C12 1.3949(17) .
C13 C14 1.5076(18) .
C15 C16 1.501(2) .
Li1 N1 1.984(2) 8_644
Li2 N2 2.018(2) 27_656
Li2 N1 2.639(2) 27_656
