#------------------------------------------------------------------------------
#$Date: 2019-11-17 09:58:04 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229227 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/64/7046419.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_7046419
loop_
_publ_author_name
'Xiao, Zhao-Xin'
'Miao, Hao'
'Shao, Dong'
'Wei, Hai-Yan'
'Zhang, Yi-Quan'
'Wang, Xin-Yi'
_publ_section_title
;
 A family of lanthanide compounds with reduced nitronyl nitroxide
 diradical: syntheses, structures and magnetic properties.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7925
_journal_page_last               7933
_journal_paper_doi               10.1039/c8dt01112e
_journal_volume                  47
_journal_year                    2018
_chemical_formula_sum            'C20 H30 N6 O4'
_chemical_formula_weight         418.50
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-03-22 deposited with the CCDC.
2018-05-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.260(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.659(4)
_cell_length_b                   14.937(9)
_cell_length_c                   10.868(6)
_cell_measurement_reflns_used    2912
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.63
_cell_measurement_theta_min      2.33
_cell_volume                     1072.3(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0235
_diffrn_reflns_av_unetI/netI     0.0298
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7173
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.626
_diffrn_reflns_theta_min         2.330
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6701
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS: Bruker, 2000'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_description       block
_exptl_crystal_F_000             448
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.230
_refine_diff_density_max         0.815
_refine_diff_density_min         -0.662
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     141
_refine_ls_number_reflns         2473
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0780
_refine_ls_R_factor_gt           0.0680
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0983P)²+1.2812P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1899
_refine_ls_wR_factor_ref         0.1995
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2067
_reflns_number_total             2473
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8dt01112e2.cif
_cod_data_source_block           NIT-Pz
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'multi-Scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7046416--7046422.cif.
;
_cod_original_cell_volume        1072.4(11)
_cod_database_code               7046419
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.975
_shelx_estimated_absorpt_t_max   0.979
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
O2 O 0.8456(3) 0.50187(11) 0.81452(15) 0.0318(4) Uani 1 1 d . .
N3 N 0.6927(3) 0.46265(12) 0.52401(16) 0.0225(4) Uani 1 1 d . .
O1 O 0.3987(3) 0.27912(13) 0.67961(19) 0.0464(6) Uani 1 1 d . U
C4 C 1.0175(3) 0.34576(15) 0.9499(2) 0.0263(5) Uani 1 1 d . .
H4A H 1.0859 0.3313 0.8798 0.039 Uiso 1 1 calc R U
H4B H 1.0378 0.2984 1.0099 0.039 Uiso 1 1 calc R U
H4C H 1.0708 0.4006 0.9866 0.039 Uiso 1 1 calc R U
N2 N 0.7628(3) 0.42510(11) 0.80474(15) 0.0180(4) Uani 1 1 d . .
N1 N 0.5514(3) 0.31781(13) 0.7386(2) 0.0343(5) Uani 1 1 d . U
C8 C 0.5536(3) 0.45242(13) 0.60124(18) 0.0196(4) Uani 1 1 d . .
C6 C 0.7919(3) 0.35667(13) 0.90753(17) 0.0184(4) Uani 1 1 d . .
C9 C 0.6411(3) 0.51067(14) 0.42022(18) 0.0209(4) Uani 1 1 d . .
C7 C 0.6201(3) 0.39856(15) 0.71407(19) 0.0233(5) Uani 1 1 d . U
C5 C 0.6860(4) 0.27346(15) 0.8424(2) 0.0302(6) Uani 1 1 d . U
C10 C 0.7957(4) 0.52084(18) 0.3327(2) 0.0312(5) Uani 1 1 d . .
H10A H 0.9284 0.5227 0.3789 0.047 Uiso 1 1 calc R U
H10B H 0.7711 0.5754 0.2866 0.047 Uiso 1 1 calc R U
H10C H 0.7868 0.4710 0.2766 0.047 Uiso 1 1 calc R U
C3 C 0.6875(4) 0.39475(18) 1.0137(2) 0.0355(6) Uani 1 1 d . .
H3A H 0.7448 0.4521 1.0377 0.053 Uiso 1 1 calc R U
H3B H 0.7069 0.3547 1.0833 0.053 Uiso 1 1 calc R U
H3C H 0.5453 0.4014 0.9869 0.053 Uiso 1 1 calc R U
C2 C 0.8317(6) 0.21236(18) 0.7817(3) 0.0506(9) Uani 1 1 d . .
H2A H 0.7556 0.1671 0.7335 0.076 Uiso 1 1 calc R U
H2B H 0.9246 0.1845 0.8450 0.076 Uiso 1 1 calc R U
H2C H 0.9059 0.2474 0.7287 0.076 Uiso 1 1 calc R U
C1 C 0.5561(5) 0.2196(2) 0.9216(3) 0.0556(10) Uani 1 1 d . .
H1A H 0.4503 0.2570 0.9454 0.083 Uiso 1 1 calc R U
H1B H 0.6388 0.1984 0.9945 0.083 Uiso 1 1 calc R U
H1C H 0.4975 0.1695 0.8747 0.083 Uiso 1 1 calc R U
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'
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
C8 N3 C9 117.68(18) . .
C6 C4 H4A 109.5 . .
C6 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
C6 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
O2 N2 C7 126.05(17) . .
O2 N2 C6 122.38(16) . .
C7 N2 C6 110.92(16) . .
O1 N1 C7 125.85(19) . .
O1 N1 C5 122.77(19) . .
C7 N1 C5 111.28(17) . .
N3 C8 C9 123.45(18) . 3_666
N3 C8 C7 115.00(18) . .
C9 C8 C7 121.55(19) 3_666 .
N2 C6 C4 109.04(17) . .
N2 C6 C3 106.17(17) . .
C4 C6 C3 109.66(18) . .
N2 C6 C5 101.30(15) . .
C4 C6 C5 115.18(18) . .
C3 C6 C5 114.7(2) . .
N3 C9 C8 118.9(2) . 3_666
N3 C9 C10 117.67(19) . .
C8 C9 C10 123.46(19) 3_666 .
N1 C7 N2 110.57(18) . .
N1 C7 C8 125.62(19) . .
N2 C7 C8 123.80(19) . .
N1 C5 C1 109.2(2) . .
N1 C5 C2 106.7(2) . .
C1 C5 C2 111.2(2) . .
N1 C5 C6 100.52(16) . .
C1 C5 C6 115.0(2) . .
C2 C5 C6 113.2(2) . .
C9 C10 H10A 109.5 . .
C9 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C9 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
C6 C3 H3A 109.5 . .
C6 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
C6 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
C5 C2 H2A 109.5 . .
C5 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
C5 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
C5 C1 H1A 109.5 . .
C5 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
C5 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O2 N2 1.271(2) .
N3 C8 1.335(3) .
N3 C9 1.344(3) .
O1 N1 1.271(3) .
C4 C6 1.523(3) .
C4 H4A 0.9600 .
C4 H4B 0.9600 .
C4 H4C 0.9600 .
N2 C7 1.340(3) .
N2 C6 1.509(2) .
N1 C7 1.329(3) .
N1 C5 1.503(3) .
C8 C9 1.401(3) 3_666
C8 C7 1.486(3) .
C6 C3 1.531(3) .
C6 C5 1.555(3) .
C9 C8 1.401(3) 3_666
C9 C10 1.495(3) .
C5 C1 1.524(4) .
C5 C2 1.540(4) .
C10 H10A 0.9600 .
C10 H10B 0.9600 .
C10 H10C 0.9600 .
C3 H3A 0.9600 .
C3 H3B 0.9600 .
C3 H3C 0.9600 .
C2 H2A 0.9600 .
C2 H2B 0.9600 .
C2 H2C 0.9600 .
C1 H1A 0.9600 .
C1 H1B 0.9600 .
C1 H1C 0.9600 .
