A new class of Dy<sup>III</sup>-SIMs associated with a guanidine-based ligand.
Ali, Basharat; Li, Xiao-Lei; Gendron, Frédéric; Le Guennic, Boris; Tang, Jinkui; Dalton transactions (Cambridge, England : 2003) 50 (2021) 5146–5153; doi:10.1039/d1dt00260k

data_7706654
_publ_section_title
;
 A new class of Dy<sup>III</sup>-SIMs associated with a guanidine-based
 ligand.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5146
_journal_page_last               5153
_journal_paper_doi               10.1039/d1dt00260k
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety
'C44 H42 Dy N12 O8, C N S, C H4 O, H2 O, 2(O), 3[H2O]'
_chemical_formula_sum            'C46 H46 Dy N13 O12 S'
_chemical_formula_weight         1167.52
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-09-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-04-26 deposited with the CCDC.	2021-02-23 downloaded from the CCDC.
;
_cell_angle_alpha                108.3410(10)
_cell_angle_beta                 102.4030(10)
_cell_angle_gamma                107.7790(10)
_cell_formula_units_Z            2
_cell_length_a                   14.1545(5)
_cell_length_b                   15.1770(5)
_cell_length_c                   15.3737(5)
_cell_measurement_reflns_used    9910
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      59.099
_cell_measurement_theta_min      4.832
_cell_volume                     2803.02(17)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0571
_diffrn_reflns_av_unetI/netI     0.0788
_diffrn_reflns_Laue_measured_fraction_full 0.957
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14655
_diffrn_reflns_point_group_measured_fraction_full 0.957
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        59.095
_diffrn_reflns_theta_max         59.095
_diffrn_reflns_theta_min         3.492
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    8.044
_exptl_absorpt_correction_T_max  0.299
_exptl_absorpt_correction_T_min  0.181
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_description       block
_exptl_crystal_F_000             1182
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.183
_refine_diff_density_min         -5.501
_refine_diff_density_rms         0.240
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.252
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     656
_refine_ls_number_reflns         7740
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.250
_refine_ls_R_factor_all          0.1068
_refine_ls_R_factor_gt           0.1029
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2696
_refine_ls_wR_factor_ref         0.2765
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7140
_reflns_number_total             7740
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00260k2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7706651--7706654.cif.'
_cod_original_cell_volume        2803.02(16)
_cod_database_code               7706654
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.378
_shelx_estimated_absorpt_t_min   0.248
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(N10) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(N3) \\sim Ueq, Uanis(C31) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(N1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C24) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O3) \\sim Ueq, Uanis(C9) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
3.a Everything fixed:
 O3, H3A, H3B
3.b Rotating group:
 O4(H4A,H4B)
3.c Aromatic/amide H refined with riding coordinates:
 N6(H6), N8(H8A), N10(H10), N12(H12), C1(H1), C3(H3), C4(H4), C8(H8B),
 C12(H12A), C14(H14), C15(H15), C16(H16), C17(H17), C20(H20), C23(H23),
 C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C32(H32),
  C33(H33), C34(H34), C35(H35), C36(H36), C38(H38), C40(H40), C41(H41),
 C42(H42), C43(H43), C44(H44), C45(H45)
3.d Idealised Me refined as rotating group:
 C46(H46A,H46B,H46C)
3.e Idealised tetrahedral OH refined as rotating group:
 O8(H8), O5(H5), O6(H6A), O7(H7), O10(H10A)
;
_shelx_res_checksum              85059
_shelx_hkl_checksum              90141
_shelx_fab_checksum              57159
_olex2_submission_special_instructions 'No special instructions were received'