#------------------------------------------------------------------------------
#$Date: 2017-06-08 08:04:40 +0300 (Thu, 08 Jun 2017) $
#$Revision: 197643 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/22/84/7228441.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_7228441
loop_
_publ_author_name
'Kong, Feng'
'Li, Meng'
'Zhou, Xigeng'
'Zhang, Lixin'
_publ_section_title
;
 Synthesis, structure and reactivity of guanidinate rare earth metal
 bis(o-aminobenzyl) complexes
;
_journal_issue                   47
_journal_name_full               'RSC Adv.'
_journal_page_first              29752
_journal_paper_doi               10.1039/C7RA04524G
_journal_volume                  7
_journal_year                    2017
_chemical_formula_sum            'C71 H82 Dy N7 S2'
_chemical_formula_weight         1260.05
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-04-04 deposited with the CCDC.
2017-05-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.312(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.114(3)
_cell_length_b                   26.401(6)
_cell_length_c                   19.568(5)
_cell_measurement_reflns_used    5016
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      25.67
_cell_measurement_theta_min      2.27
_cell_volume                     6565(3)
_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      273(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0866
_diffrn_reflns_av_unetI/netI     0.0996
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            15475
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.050
_diffrn_reflns_theta_max         25.050
_diffrn_reflns_theta_min         1.543
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.247
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.2680
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_description       block
_exptl_crystal_F_000             2620
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.300
_refine_diff_density_max         2.682
_refine_diff_density_min         -5.264
_refine_diff_density_rms         0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         5809
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0898
_refine_ls_R_factor_gt           0.0783
_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)+(0.1320P)²+0.5000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1827
_refine_ls_wR_factor_ref         0.1915
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4728
_reflns_number_total             5809
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7ra04524g2.cif
_cod_data_source_block           a60709a
_cod_database_code               7228441
_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   0.635
_shelx_estimated_absorpt_t_max   0.706
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
_atom_site_refinement_flags_occupancy
Dy1 Dy 0.5000 0.58856(2) 0.7500 0.0384(2) Uani 1 2 d S T P
S1 S 0.36655(17) 0.53194(9) 0.65039(9) 0.0684(6) Uani 1 1 d . . .
N2 N 0.5783(3) 0.66633(19) 0.7376(2) 0.0364(11) Uani 1 1 d . . .
N1 N 0.5000 0.7477(3) 0.7500 0.0478(19) Uani 1 2 d S T P
N3 N 0.3555(4) 0.5437(2) 0.7804(2) 0.0461(13) Uani 1 1 d . . .
N4 N 0.3343(8) 0.3748(4) 0.6716(6) 0.115(3) Uani 1 1 d . . .
C1 C 0.5000 0.6959(4) 0.7500 0.039(2) Uani 1 2 d S T P
C2 C 0.4058(5) 0.7790(3) 0.7491(4) 0.0568(19) Uani 1 1 d . . .
H2A H 0.4198 0.7998 0.7912 0.068 Uiso 1 1 calc R U .
H2B H 0.3473 0.7568 0.7504 0.068 Uiso 1 1 calc R U .
C3 C 0.3748(5) 0.8127(3) 0.6851(5) 0.059(2) Uani 1 1 d . . .
C4 C 0.3484(6) 0.7939(4) 0.6178(5) 0.071(2) Uani 1 1 d . . .
H4 H 0.3525 0.7591 0.6114 0.085 Uiso 1 1 calc R U .
C5 C 0.3159(6) 0.8244(5) 0.5590(5) 0.084(3) Uani 1 1 d . . .
H5 H 0.3005 0.8104 0.5140 0.101 Uiso 1 1 calc R U .
C6 C 0.3065(7) 0.8754(5) 0.5678(6) 0.088(3) Uani 1 1 d . . .
H6 H 0.2823 0.8961 0.5287 0.106 Uiso 1 1 calc R U .
C7 C 0.3323(10) 0.8956(4) 0.6327(7) 0.096(3) Uani 1 1 d . . .
H7 H 0.3282 0.9305 0.6383 0.115 Uiso 1 1 calc R U .
C8 C 0.3653(8) 0.8644(4) 0.6921(5) 0.079(3) Uani 1 1 d . . .
H8 H 0.3809 0.8788 0.7368 0.095 Uiso 1 1 calc R U .
C9 C 0.6565(4) 0.6792(2) 0.7007(3) 0.0372(14) Uani 1 1 d . . .
C10 C 0.7641(4) 0.6795(3) 0.7389(4) 0.0484(16) Uani 1 1 d . . .
C11 C 0.8400(4) 0.6859(3) 0.7013(4) 0.063(2) Uani 1 1 d . . .
H11 H 0.9106 0.6857 0.7256 0.075 Uiso 1 1 calc R U .
C12 C 0.8145(5) 0.6924(4) 0.6297(5) 0.072(2) Uani 1 1 d . . .
H12 H 0.8672 0.6972 0.6061 0.086 Uiso 1 1 calc R U .
C13 C 0.7102(5) 0.6918(3) 0.5928(4) 0.061(2) Uani 1 1 d . . .
H13 H 0.6930 0.6956 0.5440 0.073 Uiso 1 1 calc R U .
C14 C 0.6311(4) 0.6858(3) 0.6273(3) 0.0462(16) Uani 1 1 d . . .
C15 C 0.7972(5) 0.6730(4) 0.8179(4) 0.065(2) Uani 1 1 d . . .
H15 H 0.7339 0.6720 0.8359 0.077 Uiso 1 1 calc R U .
C16 C 0.8585(8) 0.6240(4) 0.8387(5) 0.100(3) Uani 1 1 d . . .
H16A H 0.8185 0.5961 0.8145 0.149 Uiso 1 1 calc R U .
H16B H 0.8712 0.6191 0.8887 0.149 Uiso 1 1 calc R U .
H16C H 0.9245 0.6260 0.8259 0.149 Uiso 1 1 calc R U .
C17 C 0.8657(6) 0.7181(4) 0.8526(5) 0.093(3) Uani 1 1 d . . .
H17A H 0.9328 0.7165 0.8414 0.140 Uiso 1 1 calc R U .
H17B H 0.8755 0.7165 0.9028 0.140 Uiso 1 1 calc R U .
H17C H 0.8312 0.7493 0.8351 0.140 Uiso 1 1 calc R U .
C18 C 0.5182(4) 0.6823(3) 0.5837(3) 0.0518(17) Uani 1 1 d . . .
H18 H 0.4726 0.6900 0.6152 0.062 Uiso 1 1 calc R U .
C19 C 0.4919(7) 0.7204(4) 0.5228(4) 0.082(3) Uani 1 1 d . . .
H19A H 0.5271 0.7107 0.4873 0.124 Uiso 1 1 calc R U .
H19B H 0.5148 0.7535 0.5402 0.124 Uiso 1 1 calc R U .
H19C H 0.4172 0.7207 0.5029 0.124 Uiso 1 1 calc R U .
C20 C 0.4924(6) 0.6293(4) 0.5563(5) 0.077(3) Uani 1 1 d . . .
H20A H 0.5304 0.6219 0.5214 0.116 Uiso 1 1 calc R U .
H20B H 0.4182 0.6267 0.5354 0.116 Uiso 1 1 calc R U .
H20C H 0.5121 0.6056 0.5945 0.116 Uiso 1 1 calc R U .
C21 C 0.3289(5) 0.5148(3) 0.7271(3) 0.0530(17) Uani 1 1 d . . .
C22 C 0.2708(10) 0.4657(4) 0.7291(5) 0.098(4) Uani 1 1 d . . .
H22A H 0.2239 0.4707 0.7599 0.118 Uiso 1 1 calc R U .
H22B H 0.3222 0.4405 0.7513 0.118 Uiso 1 1 calc R U .
C23 C 0.2065(7) 0.4434(4) 0.6607(4) 0.069(2) Uani 1 1 d . . .
C24 C 0.2366(9) 0.3979(4) 0.6359(5) 0.081(3) Uani 1 1 d . . .
C25 C 0.1692(12) 0.3752(5) 0.5787(6) 0.114(5) Uani 1 1 d . . .
H25 H 0.1882 0.3445 0.5621 0.136 Uiso 1 1 calc R U .
C26 C 0.0772(15) 0.3963(9) 0.5467(8) 0.158(9) Uani 1 1 d . . .
H26 H 0.0318 0.3796 0.5095 0.190 Uiso 1 1 calc R U .
C27 C 0.0496(11) 0.4427(9) 0.5686(10) 0.155(7) Uani 1 1 d . . .
H27 H -0.0124 0.4584 0.5446 0.186 Uiso 1 1 calc R U .
C28 C 0.1137(9) 0.4652(6) 0.6254(7) 0.119(4) Uani 1 1 d . . .
H28 H 0.0942 0.4962 0.6409 0.143 Uiso 1 1 calc R U .
C29 C 0.4228(14) 0.3907(7) 0.6462(14) 0.219(12) Uani 1 1 d . . .
H29A H 0.4848 0.3733 0.6718 0.329 Uiso 1 1 calc R U .
H29B H 0.4325 0.4266 0.6529 0.329 Uiso 1 1 calc R U .
H29C H 0.4103 0.3829 0.5969 0.329 Uiso 1 1 calc R U .
C30 C 0.3359(15) 0.3219(7) 0.6805(14) 0.227(12) Uani 1 1 d . . .
H30A H 0.3840 0.3072 0.6564 0.340 Uiso 1 1 calc R U .
H30B H 0.2666 0.3086 0.6615 0.340 Uiso 1 1 calc R U .
H30C H 0.3581 0.3140 0.7299 0.340 Uiso 1 1 calc R U .
C31 C 0.3231(5) 0.5334(3) 0.8442(3) 0.0460(15) Uani 1 1 d . . .
C32 C 0.2355(6) 0.5567(3) 0.8552(4) 0.064(2) Uani 1 1 d . . .
H32 H 0.1958 0.5777 0.8205 0.077 Uiso 1 1 calc R U .
C33 C 0.2053(7) 0.5496(4) 0.9168(4) 0.075(3) Uani 1 1 d . . .
H33 H 0.1447 0.5652 0.9230 0.090 Uiso 1 1 calc R U .
C34 C 0.2627(6) 0.5200(3) 0.9686(4) 0.066(2) Uani 1 1 d . . .
H34 H 0.2421 0.5155 1.0104 0.079 Uiso 1 1 calc R U .
C35 C 0.3510(6) 0.4967(3) 0.9591(3) 0.0590(19) Uani 1 1 d . . .
H35 H 0.3907 0.4766 0.9949 0.071 Uiso 1 1 calc R U .
C36 C 0.3824(5) 0.5027(3) 0.8972(4) 0.0564(19) Uani 1 1 d . . .
H36 H 0.4424 0.4864 0.8910 0.068 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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 '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 Dy1 N2 56.9(2) . 2_656
N2 Dy1 N3 147.51(17) . .
N2 Dy1 N3 90.78(17) 2_656 .
N2 Dy1 N3 90.78(17) . 2_656
N2 Dy1 N3 147.51(18) 2_656 2_656
N3 Dy1 N3 121.7(3) . 2_656
N2 Dy1 S1 109.64(12) . 2_656
N2 Dy1 S1 129.03(12) 2_656 2_656
N3 Dy1 S1 87.66(14) . 2_656
N3 Dy1 S1 60.37(12) 2_656 2_656
N2 Dy1 S1 129.03(12) . .
N2 Dy1 S1 109.64(12) 2_656 .
N3 Dy1 S1 60.37(12) . .
N3 Dy1 S1 87.66(14) 2_656 .
S1 Dy1 S1 113.38(11) 2_656 .
N2 Dy1 C1 28.43(10) . .
N2 Dy1 C1 28.43(10) 2_656 .
N3 Dy1 C1 119.16(14) . .
N3 Dy1 C1 119.17(14) 2_656 .
S1 Dy1 C1 123.31(6) 2_656 .
S1 Dy1 C1 123.31(6) . .
N2 Dy1 C21 155.67(19) . .
N2 Dy1 C21 105.17(18) 2_656 .
N3 Dy1 C21 25.41(17) . .
N3 Dy1 C21 104.7(2) 2_656 .
S1 Dy1 C21 94.42(16) 2_656 .
S1 Dy1 C21 35.95(13) . .
C1 Dy1 C21 131.82(16) . .
N2 Dy1 C21 105.17(18) . 2_656
N2 Dy1 C21 155.67(19) 2_656 2_656
N3 Dy1 C21 104.7(2) . 2_656
N3 Dy1 C21 25.41(17) 2_656 2_656
S1 Dy1 C21 35.95(13) 2_656 2_656
S1 Dy1 C21 94.42(16) . 2_656
C1 Dy1 C21 131.82(16) . 2_656
C21 Dy1 C21 96.4(3) . 2_656
C21 S1 Dy1 78.2(2) . .
C1 N2 C9 128.3(6) . .
C1 N2 Dy1 96.7(4) . .
C9 N2 Dy1 130.5(4) . .
C1 N1 C2 123.9(4) . 2_656
C1 N1 C2 123.9(4) . .
C2 N1 C2 112.2(8) 2_656 .
C21 N3 C31 121.2(6) . .
C21 N3 Dy1 99.5(4) . .
C31 N3 Dy1 136.0(4) . .
C30 N4 C29 110.2(14) . .
C30 N4 C24 117.8(12) . .
C29 N4 C24 114.1(12) . .
N2 C1 N2 109.8(8) 2_656 .
N2 C1 N1 125.1(4) 2_656 .
N2 C1 N1 125.1(4) . .
N2 C1 Dy1 54.9(4) 2_656 .
N2 C1 Dy1 54.9(4) . .
N1 C1 Dy1 180.0 . .
N1 C2 C3 113.1(5) . .
C4 C3 C8 116.5(8) . .
C4 C3 C2 122.4(8) . .
C8 C3 C2 121.0(8) . .
C3 C4 C5 122.7(9) . .
C6 C5 C4 119.2(10) . .
C7 C6 C5 120.1(10) . .
C6 C7 C8 120.2(11) . .
C3 C8 C7 121.1(10) . .
C14 C9 C10 119.3(5) . .
C14 C9 N2 121.8(5) . .
C10 C9 N2 118.4(5) . .
C11 C10 C9 118.1(6) . .
C11 C10 C15 119.6(5) . .
C9 C10 C15 122.3(5) . .
C12 C11 C10 122.2(6) . .
C11 C12 C13 119.6(6) . .
C14 C13 C12 120.9(7) . .
C13 C14 C9 119.9(6) . .
C13 C14 C18 118.6(6) . .
C9 C14 C18 121.3(5) . .
C10 C15 C16 111.6(7) . .
C10 C15 C17 110.7(8) . .
C16 C15 C17 109.0(7) . .
C20 C18 C14 111.0(6) . .
C20 C18 C19 110.1(7) . .
C14 C18 C19 113.5(6) . .
N3 C21 C22 122.2(6) . .
N3 C21 S1 118.0(5) . .
C22 C21 S1 119.7(5) . .
N3 C21 Dy1 55.1(3) . .
C22 C21 Dy1 160.5(7) . .
S1 C21 Dy1 65.8(2) . .
C21 C22 C23 119.0(7) . .
C28 C23 C24 118.8(10) . .
C28 C23 C22 120.9(11) . .
C24 C23 C22 120.1(10) . .
C25 C24 C23 118.6(12) . .
C25 C24 N4 121.8(12) . .
C23 C24 N4 119.6(9) . .
C26 C25 C24 121.5(14) . .
C25 C26 C27 120.1(14) . .
C28 C27 C26 119.2(17) . .
C27 C28 C23 121.6(16) . .
C32 C31 C36 118.8(6) . .
C32 C31 N3 119.4(6) . .
C36 C31 N3 121.7(6) . .
C31 C32 C33 120.9(7) . .
C34 C33 C32 120.7(7) . .
C33 C34 C35 119.5(6) . .
C34 C35 C36 121.0(7) . .
C35 C36 C31 119.1(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Dy1 N2 2.335(5) .
Dy1 N2 2.335(5) 2_656
Dy1 N3 2.430(5) .
Dy1 N3 2.430(5) 2_656
Dy1 S1 2.7221(19) 2_656
Dy1 S1 2.7221(19) .
Dy1 C1 2.835(10) .
Dy1 C21 2.921(7) .
Dy1 C21 2.921(7) 2_656
S1 C21 1.752(6) .
N2 C1 1.359(7) .
N2 C9 1.433(7) .
N1 C1 1.365(12) .
N1 C2 1.482(8) 2_656
N1 C2 1.482(7) .
N3 C21 1.270(8) .
N3 C31 1.441(7) .
N4 C30 1.406(18) .
N4 C29 1.433(16) .
N4 C24 1.434(15) .
C1 N2 1.359(7) 2_656
C2 C3 1.508(11) .
C3 C4 1.370(12) .
C3 C8 1.380(12) .
C4 C5 1.384(13) .
C5 C6 1.365(15) .
C6 C7 1.342(16) .
C7 C8 1.403(14) .
C9 C14 1.403(9) .
C9 C10 1.424(7) .
C10 C11 1.387(9) .
C10 C15 1.509(10) .
C11 C12 1.369(11) .
C12 C13 1.380(10) .
C13 C14 1.380(8) .
C14 C18 1.517(8) .
C15 C16 1.525(14) .
C15 C17 1.543(12) .
C18 C20 1.507(12) .
C18 C19 1.532(10) .
C21 C22 1.509(12) .
C22 C23 1.513(12) .
C23 C28 1.369(16) .
C23 C24 1.389(14) .
C24 C25 1.380(15) .
C25 C26 1.34(2) .
C26 C27 1.38(3) .
C27 C28 1.35(2) .
C31 C32 1.368(10) .
C31 C36 1.392(10) .
C32 C33 1.372(10) .
C33 C34 1.350(12) .
C34 C35 1.363(11) .
C35 C36 1.381(9) .
