#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:50:37 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179992 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/86/7028665.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_7028665
loop_
_publ_author_name
'De Almeida, Lucie'
'Grandjean, Stéphane'
'Rivenet, Murielle'
'Patisson, Fabrice'
'Abraham, Francis'
_publ_section_title
;
 Hydrazinium lanthanide oxalates: synthesis, structure and thermal
 reactivity of N2H5[Ln2(C2O4)4(N2H5)]·4H2O, Ln = Ce, Nd.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4680
_journal_page_last               4688
_journal_paper_doi               10.1039/c3dt52944d
_journal_volume                  43
_journal_year                    2014
_chemical_formula_sum            'C8 H18 N4 Nd2 O20'
_chemical_formula_weight         778.7
_chemical_name_systematic        ' ?'
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_cell_angle_alpha                90
_cell_angle_beta                 116.638(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.315(4)
_cell_length_b                   12.127(3)
_cell_length_c                   11.430(2)
_cell_measurement_reflns_used    9149
_cell_measurement_temperature    296
_cell_measurement_theta_max      34.96
_cell_measurement_theta_min      2.50
_cell_volume                     2021.4(8)
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.96
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0578
_diffrn_reflns_av_sigmaI/netI    0.0372
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            47511
_diffrn_reflns_theta_full        35.65
_diffrn_reflns_theta_max         39.55
_diffrn_reflns_theta_min         1.99
_exptl_absorpt_coefficient_mu    5.191
_exptl_absorpt_correction_T_max  0.7478
_exptl_absorpt_correction_T_min  0.6527
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'pale violet'
_exptl_crystal_density_diffrn    2.558
_exptl_crystal_description       plate
_exptl_crystal_F_000             1468
_exptl_crystal_size_max          0.077
_exptl_crystal_size_mid          0.047
_exptl_crystal_size_min          0.005
_refine_diff_density_max         0.10
_refine_diff_density_min         -0.19
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_gt    2.28
_refine_ls_goodness_of_fit_ref   1.98
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_constraints    26
_refine_ls_number_parameters     174
_refine_ls_number_reflns         5984
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0313
_refine_ls_shift/su_max          0.0362
_refine_ls_shift/su_mean         0.0016
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     w=1/σ²(F)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0295
_refine_ls_wR_factor_ref         0.0306
_reflns_number_gt                4231
_reflns_number_total             5984
_reflns_threshold_expression     I>3σ(I)
_cod_data_source_file            c3dt52944d.txt
_cod_data_source_block           (I)
_cod_original_cell_volume        2021.4(7)
_cod_database_code               7028665
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,y,-z
3 -x,-y,-z
4 x,-y,z
5 1/2+x,1/2+y,z
6 1/2-x,1/2+y,-z
7 1/2-x,1/2-y,-z
8 1/2+x,1/2-y,z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_adp_type
_atom_site_U_iso_or_equiv
_atom_site_symmetry_multiplicity
_atom_site_occupancy
_atom_site_calc_flag
Nd1 Nd 0.109653(14) 0 0.19499(2) Uani 0.01394(7) 4 1 d
Nd2 Nd 0.286967(14) 0 0.81338(2) Uani 0.01410(7) 4 1 d
O2 O 0.19962(19) 0 0.9427(3) Uani 0.0216(11) 4 1 d
O1 O -0.06312(19) 0 0.0523(3) Uani 0.0189(10) 4 1 d
O4 O 0.1177(2) 0 0.6848(3) Uani 0.0263(12) 4 1 d
O3 O 0.01818(20) 0 0.3165(3) Uani 0.0272(12) 4 1 d
C1 C 0.1141(3) 0 0.8920(4) Uani 0.0156(13) 4 1 d
O5 O 0.05132(14) 0.19281(16) 0.1530(2) Uani 0.0231(8) 8 1 d
O6 O 0.41524(13) 0.13053(16) 0.8591(2) Uani 0.0224(8) 8 1 d
C3 C 0.10198(18) 0.2687(2) 0.1482(3) Uani 0.0166(9) 8 1 d
O8 O 0.25838(15) 0.19098(16) 0.8608(2) Uani 0.0263(9) 8 1 d
O7 O 0.21369(14) 0.13326(16) 0.1660(2) Uani 0.0224(8) 8 1 d
N1 N 0.4011(3) 0 1.0721(4) Uani 0.0284(16) 4 1 d
C4 C 0.30636(19) 0.2663(2) 0.8490(3) Uani 0.0172(10) 8 1 d
C2 C -0.0659(3) 0 0.2591(4) Uani 0.0197(14) 4 1 d
O10 O 0.25176(16) -0.10982(17) 0.6158(2) Uani 0.0287(9) 8 1 d
O9 O 0.19382(18) 0.10943(18) 0.3983(2) Uani 0.0352(10) 8 1 d
N2 N 0.3670(3) 0 1.1700(4) Uani 0.0332(16) 4 1 d
C5 C 0.2233(2) 0.0634(2) 0.5068(3) Uani 0.0220(10) 8 1 d
Ow1 O 0.08242(19) 0.2691(3) 0.7809(4) Uani 0.0518(15) 8 1 d
Ow2 O 0.5295(4) 0 1.3904(6) Uani 0.088(3) 4 1 d
N3 N 0.6108(3) 0.2102(3) 1.4976(4) Uiso 0.0746(12) 8 0.5 d
Ow3 O 0.6108(3) 0.2102(3) 1.4976(4) Uiso 0.0746(12) 8 0.5 d
N4 N 0.5381(4) 0.2939(5) 1.4960(7) Uiso 0.0449(16) 8 0.5 d
H1n1 H 0.441571 -0.052146 1.089747 Uiso 0.0341 8 1 d
H1n2 H 0.413097 0 1.247861 Uiso 0.0398 4 1 d
H2n2 H 0.333796 0.058575 1.16036 Uiso 0.0398 8 1 d
H1ow2 H 0.556(4) -0.059(3) 1.402(6) Uiso 0.132 8 1 d
H1ow1 H 0.048(3) 0.249(4) 0.813(5) Uiso 0.0777 8 1 d
H2ow1 H 0.1339(15) 0.242(4) 0.820(4) Uiso 0.0777 8 1 d
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
C 0.0033 0.0016 'International Tables Vol C tables 4.2.6.8 and 6.1.1.4' 2.31
20.843901 1.02 10.2075 1.5886 0.5687 0.865 51.651199 0.2156
H 0.0000 0.0000 'International Tables Vol C tables 4.2.6.8 and 6.1.1.4'
0.493002 10.5109 0.322912 26.1257 0.140191 3.14236 0.04081 57.799702 0.003038
N 0.0061 0.0033 'International Tables Vol C tables 4.2.6.8 and 6.1.1.4' 12.2126
0.0057 3.1322 9.8933 2.0125 28.997499 1.1663 0.5826 -11.529
Nd -0.1943 3.0179 'International Tables Vol C tables 4.2.6.8 and 6.1.1.4'
22.6845 2.66248 19.6847 0.210628 12.774 15.885 2.85137 137.903 1.98486
O 0.0106 0.0060 'International Tables Vol C tables 4.2.6.8 and 6.1.1.4' 3.0485
13.2771 2.2868 5.7011 1.5463 0.3239 0.867 32.908901 0.2508
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Nd1 O1 . 2.546(3)
Nd1 O1 2_555 2.577(3)
Nd1 O3 . 2.452(4)
Nd1 O5 . 2.489(2)
Nd1 O5 4_555 2.489(2)
Nd1 O7 . 2.471(2)
Nd1 O7 4_555 2.471(2)
Nd1 O9 . 2.487(2)
Nd1 O9 4_555 2.487(2)
Nd2 O2 . 2.471(4)
Nd2 O4 . 2.479(3)
Nd2 O6 . 2.486(2)
Nd2 O6 4_555 2.486(2)
Nd2 O8 . 2.470(2)
Nd2 O8 4_555 2.470(2)
Nd2 N1 . 2.697(4)
Nd2 O10 . 2.458(2)
Nd2 O10 4_555 2.458(2)
C1 O2 . 1.248(5)
C1 O1 2_556 1.254(6)
C1 O4 . 2.396(6)
C1 O3 2_556 2.393(4)
C3 O5 . 1.255(4)
C3 O6 7_556 1.248(3)
C3 O8 7_556 2.377(4)
C3 O7 . 2.393(4)
N1 N2 . 1.456(7)
C4 O5 7_556 2.384(4)
C4 O6 . 2.387(4)
C4 O8 . 1.250(4)
C4 O7 7_556 1.252(3)
C2 O2 2_556 2.359(4)
C2 O1 . 2.385(6)
C2 O4 2_556 1.269(7)
C2 O3 . 1.228(5)
C5 O10 . 2.380(4)
C5 O10 4_555 1.252(4)
C5 O9 . 1.243(4)
C5 O9 4_555 2.372(4)
N3 N4 . 1.555(9)
N3 N4 2_658 2.665(9)
N4 N4 2_658 1.288(11)
