Solvent responses and substituent effects upon magnetic properties of mononuclear Dy<sup>III</sup> compounds.
Zhang, Sheng; Shen, Nan; Zhang, Jiangwei; Xu, Fang; Zhang, Jin; Tang, Jiamin; Hu, Dengwei; Yin, Bing; Chen, Sanping; Dalton transactions (Cambridge, England : 2003) 50 (2021) 624–637; doi:10.1039/d0dt03477k

data_7705819
_publ_section_title
;
 Solvent responses and substituent effects upon magnetic properties of
 mononuclear Dy<sup>III</sup> compounds.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              624
_journal_page_last               637
_journal_paper_doi               10.1039/d0dt03477k
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C52 H53 Dy N4 O7'
_chemical_formula_sum            'C52 H53 Dy N4 O7'
_chemical_formula_weight         1008.48
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-12-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-03-23 deposited with the CCDC.	2020-11-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.711(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   31.8719(6)
_cell_length_b                   10.4645(2)
_cell_length_c                   33.4231(7)
_cell_measurement_reflns_used    13710
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      75.8330
_cell_measurement_theta_min      2.9270
_cell_volume                     9957.8(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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     38.00  89.00   1.00    6.50    --  106.49-105.00 138.00   51
  2  \w     19.00  79.00   1.00    0.70    --   48.45-105.00 138.00   60
  3  \w     92.00 175.00   1.00    6.50    --  106.49  57.00  60.00   83
  4  \w     92.00 176.00   1.00    6.50    --  106.49  57.00  30.00   84
  5  \w    103.00 129.00   1.00    6.50    --  106.49 105.00-121.00   26
  6  \w     95.00 177.00   1.00    6.50    --  106.49 125.00-150.00   82
  7  \w     34.00  97.00   1.00    6.50    --  106.49 -99.00-120.00   63
  8  \w     34.00 111.00   1.00    6.50    --  106.49-125.00-120.00   77
  9  \w    -27.00   0.00   1.00    0.70    --  -48.45 105.00-121.00   27
 10  \w    -63.00  21.00   1.00    0.70    --  -48.45  57.00   0.00   84
 11  \w    -64.00 -21.00   1.00    6.50    --  -86.25 105.00-121.00   43
 12  \w    -83.00 -48.00   1.00    0.70    --  -48.45 105.00-121.00   35
 13  \w   -151.00 -85.00   1.00    6.50    --  -86.25 -38.00-180.00   66
 14  \w   -116.00 -70.00   1.00    0.70    --  -48.45-125.00 -60.00   46
 15  \w   -144.00-119.00   1.00    6.50    --  -86.25-105.00 138.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0159394000
_diffrn_orient_matrix_UB_12      -0.1405358000
_diffrn_orient_matrix_UB_13      0.0083652000
_diffrn_orient_matrix_UB_21      -0.0313436000
_diffrn_orient_matrix_UB_22      -0.0222022000
_diffrn_orient_matrix_UB_23      0.0234979000
_diffrn_orient_matrix_UB_31      -0.0411453000
_diffrn_orient_matrix_UB_32      -0.0376816000
_diffrn_orient_matrix_UB_33      -0.0451676000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0423
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            28463
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.076
_diffrn_reflns_theta_max         67.076
_diffrn_reflns_theta_min         2.960
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    8.454
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.06829
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.25a (Rigaku Oxford Diffraction, 2018)
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    1.345
_exptl_crystal_description       block
_exptl_crystal_F_000             4120
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.021
_refine_diff_density_min         -0.820
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     583
_refine_ls_number_reflns         8771
_refine_ls_number_restraints     73
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0695
_refine_ls_R_factor_gt           0.0575
_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^)+(0.0923P)^2^+34.2347P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1543
_refine_ls_wR_factor_ref         0.1720
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7377
_reflns_number_total             8771
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03477k2.cif
_cod_data_source_block           191213a
_cod_depositor_comments
'Adding full bibliography for 7705816--7705819.cif.'
_cod_database_code               7705819
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         DyCNO
_shelx_estimated_absorpt_t_max   0.849
_shelx_estimated_absorpt_t_min   0.677
_reflns_odcompleteness_completeness 98.46
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Restrained distances
 C52-C51
 2.35 with sigma of 0.01
 C52-C50
 2.35 with sigma of 0.01
 C51-C50
 2.35 with sigma of 0.01
 C49-C44 = C49-C50 = C49-C51 = C49-C52
 1.55 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C6 \\sim C12 \\sim C17 \\sim C32 \\sim C36 \\sim C43 \\sim C44 \\sim C49 \\sim
C50 \\sim C51 \\sim C52: within 2A with sigma of 0.004 and sigma for terminal
atoms of 0.008
4.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C8(H8A,H8B), C9(H9A,H9B), C22(H22A,H22B), C30(H30A,
 H30B)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C6(H6), C11(H11), C18(H18), C20(H20), C25(H25), C26(H26), C27(H27),
 C28(H28), C29(H29), C31(H31), C32(H32), C34(H34), C35(H35), C36(H36), C37(H37),
  C38(H38), C40(H40), C41(H41), C42(H42), C43(H43), C46(H46), C47(H47)
4.c Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C45(H45A,H45B,H45C), C48(H48A,H48B,H48C), C50(H50A,H50B,
 H50C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C)
;
_shelx_res_checksum              58221
_shelx_fab_checksum              21927
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 8.607
_oxdiff_exptl_absorpt_empirical_full_min 0.459