A neutral auxiliary ligand enhanced dysprosium(iii) single molecule magnet.
Chen, Xiao-Xiang; Ma, Fang; Xu, Mei-Xing; Bi, Jin-Cheng; Sun, Hao-Ling; Wang, Bing-Wu; Gao, Song; Dalton transactions (Cambridge, England : 2003) 47 (2018) 7395–7398; doi:10.1039/c8dt01102h

data_7046289
_publ_section_title
;
 A neutral auxiliary ligand enhanced dysprosium(iii) single molecule
 magnet.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7395
_journal_page_last               7398
_journal_paper_doi               10.1039/c8dt01102h
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C38 H66 Dy N7 Si2'
_chemical_formula_sum            'C38 H66 Dy N7 Si2'
_chemical_formula_weight         839.65
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-04-11
_audit_creation_method
;
Olex2 1.2
(compiled 2017.02.23 svn.r3390 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2018-04-18 deposited with the CCDC.
2018-05-09 downloaded from the CCDC.
;
_cell_angle_alpha                88.619(2)
_cell_angle_beta                 80.960(2)
_cell_angle_gamma                69.139(2)
_cell_formula_units_Z            2
_cell_length_a                   10.7692(3)
_cell_length_b                   10.8103(3)
_cell_length_c                   19.6786(5)
_cell_measurement_reflns_used    23073
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      30.3170
_cell_measurement_theta_min      3.6500
_cell_volume                     2112.92(10)
_computing_cell_refinement       'CrysAlisPro 1.171.39.16b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.16b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.16b (Rigaku OD, 2015)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      180.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -12.00  27.00   0.50    1.00    --   -1.60 -82.00  60.00   78
  2  \w    -46.00 -19.00   0.50    1.00    --   -1.60 -77.00-150.00   54
  3  \w    -91.00 -31.00   0.50    1.00    --   -1.60 -19.00   0.00  120
  4  \w    -33.00  31.00   0.50    1.00    --   -1.60 -82.00 120.00  128
  5  \w    -18.00   9.00   0.50    1.00    --   -1.60 -82.00 -90.00   54
  6  \w    -29.00  30.00   0.50    1.00    --   -1.60 -82.00-150.00  118
  7  \w    -41.00  32.00   0.50    1.00    --    1.90 -77.00   0.00  146
  8  \w    -85.00 -27.00   0.50    1.00    --    1.90 -57.00 -60.00  116
  9  \w     48.00  88.00   0.50    1.00    --    1.90  57.00-120.00   80
 10  \w    -15.00  10.00   0.50    1.00    --    1.90  57.00-120.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0693437000
_diffrn_orient_matrix_UB_12      0.0314182000
_diffrn_orient_matrix_UB_13      0.0131910000
_diffrn_orient_matrix_UB_21      -0.0032478000
_diffrn_orient_matrix_UB_22      0.0530646000
_diffrn_orient_matrix_UB_23      -0.0224085000
_diffrn_orient_matrix_UB_31      -0.0166670000
_diffrn_orient_matrix_UB_32      -0.0336635000
_diffrn_orient_matrix_UB_33      -0.0256421000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0261
_diffrn_reflns_av_unetI/netI     0.0225
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            38779
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.877
_diffrn_reflns_theta_min         3.472
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.859
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.544
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.16b (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_description       block
_exptl_crystal_F_000             874
_exptl_crystal_size_max          0.298
_exptl_crystal_size_mid          0.179
_exptl_crystal_size_min          0.143
_refine_diff_density_max         0.814
_refine_diff_density_min         -0.554
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         9965
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0195
_refine_ls_R_factor_gt           0.0180
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0215P)^2^+0.6694P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0446
_refine_ls_wR_factor_ref         0.0451
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9470
_reflns_number_total             9965
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01102h2.cif
_cod_data_source_block           2
_cod_depositor_comments          'Adding full bibliography for 7046289.cif.'
_cod_database_code               7046289
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'C38 H66 Dy N7 Si2'
_chemical_oxdiff_usercomment     DyLNstar2
_reflns_odcompleteness_completeness 99.60
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{C8A, C8B}
{C1A, C1B}
3. Restrained distances
 C36A-C37A \\sim C37A-C38A \\sim C36A-C38A
 with sigma of 0.04
 C36B-C37B \\sim C37B-C38B \\sim C36B-C38B
 with sigma of 0.04
 Si2-C36A \\sim Si2-C36B \\sim Si2-C37A \\sim Si2-C37B \\sim Si2-C38A \\sim
Si2-C38B
 with sigma of 0.02
 N7-C36A \\sim N7-C37A \\sim N7-C38A \\sim N7-C36B \\sim N7-C37B \\sim N7-C38B
 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
Uanis(C37B) \\sim Ueq, Uanis(C38B) \\sim Ueq, Uanis(C36B) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C8A) = Uanis(C8B)
Uanis(C1A) = Uanis(C1B)
5. Others
 Sof(C36B)=Sof(H36D)=Sof(H36E)=Sof(H36F)=Sof(C37B)=Sof(H37D)=Sof(H37E)=
 Sof(H37F)=Sof(C38B)=Sof(H38D)=Sof(H38E)=Sof(H38F)=1-FVAR(1)
 Sof(C38A)=Sof(H38A)=Sof(H38B)=Sof(H38C)=Sof(C36A)=Sof(H36A)=Sof(H36B)=
 Sof(H36C)=Sof(C37A)=Sof(H37A)=Sof(H37B)=Sof(H37C)=FVAR(1)
 Sof(C0AA)=Sof(H0AA)=Sof(H0AB)=Sof(C8B)=Sof(H8BA)=Sof(H8BB)=Sof(C1B)=Sof(H1BA)=
 Sof(H1BB)=Sof(H1BC)=1-FVAR(2)
 Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(C7)=
 Sof(H7A)=Sof(H7B)=FVAR(2)
6.a Riding coordinates:
 C4(H4), C3(H3), C1A(H1AA,H1AB,H1AC), C14(H14), C1B(H1BA,H1BB,H1BC)
6.b Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C24(H24A,H24B), C25(H25A,H25B), C9(H9A,H9B), C10(H10A,H10B),
 C23(H23A,H23B), C8A(H8AA,H8AB), C7(H7A,H7B), C0AA(H0AA,H0AB), C8B(H8BA,H8BB)
6.c Aromatic/amide H refined with riding coordinates:
 C29(H29), C13(H13), C30(H30), C20(H20), C19(H19)
6.d Idealised Me refined as rotating group:
 C38A(H38A,H38B,H38C), C36A(H36A,H36B,H36C), C37A(H37A,H37B,H37C), C6(H6A,H6B,
 H6C), C34(H34A,H34B,H34C), C33(H33A,H33B,H33C), C35(H35A,H35B,H35C), C27(H27A,
 H27B,H27C), C11(H11A,H11B,H11C), C22(H22A,H22B,H22C), C16(H16A,H16B,H16C),
 C17(H17A,H17B,H17C), C32(H32A,H32B,H32C), C36B(H36D,H36E,H36F), C37B(H37D,H37E,
 H37F), C38B(H38D,H38E,H38F)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.607
_oxdiff_exptl_absorpt_empirical_full_min 0.731