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_7705816
_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         'C49 H47 Dy N4 O8, C4 H8 O2'
_chemical_formula_sum            'C53 H55 Dy N4 O10'
_chemical_formula_weight         1070.51
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-12-20
_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                 95.0790(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.7403(2)
_cell_length_b                   10.2716(2)
_cell_length_c                   28.7185(4)
_cell_measurement_reflns_used    11333
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      76.3990
_cell_measurement_theta_min      3.1420
_cell_volume                     4918.75(13)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_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 0.970
_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    -68.00  15.00   1.00    0.20    --  -48.45  73.00-164.00   83
  2  \w   -110.00 -27.00   1.00    0.20    --  -48.45 -73.00  65.00   83
  3  \w     50.00  75.00   1.00    0.20    --   48.45  73.00-164.00   25
  4  \w    -23.00  39.00   1.00    0.20    --   48.45 -73.00  65.00   62
  5  \w   -120.00 -71.00   1.00    0.20    --  -48.45-125.00 120.00   49
  6  \w    -64.00 -19.00   1.00    1.40    --  -86.25  73.00-164.00   45
  7  \w   -109.00 -15.00   1.00    1.40    --  -86.25  77.00  30.00   94
  8  \w     34.00 127.00   1.00    1.40    --  106.49 -73.00  65.00   93
  9  \w     89.00 131.00   1.00    1.40    --  106.49  73.00-164.00   42
 10  \w     91.00 178.00   1.00    1.40    --  106.49  77.00 120.00   87
 11  \w     92.00 176.00   1.00    1.40    --  106.49  57.00-180.00   84
 12  \w     96.00 177.00   1.00    1.40    --  106.49  38.00 120.00   81
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0755773000
_diffrn_orient_matrix_UB_12      -0.0783915000
_diffrn_orient_matrix_UB_13      -0.0167488000
_diffrn_orient_matrix_UB_21      -0.0152916000
_diffrn_orient_matrix_UB_22      0.0919614000
_diffrn_orient_matrix_UB_23      -0.0422539000
_diffrn_orient_matrix_UB_31      0.0508839000
_diffrn_orient_matrix_UB_32      -0.0888032000
_diffrn_orient_matrix_UB_33      -0.0289083000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0497
_diffrn_reflns_av_unetI/netI     0.0471
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            27683
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.077
_diffrn_reflns_theta_min         2.947
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.639
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49456
_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    1.446
_exptl_crystal_description       block
_exptl_crystal_F_000             2188
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.443
_refine_diff_density_min         -0.473
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     617
_refine_ls_number_reflns         8651
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0544
_refine_ls_R_factor_gt           0.0382
_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^)+(0.0342P)^2^+5.0134P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0859
_refine_ls_wR_factor_ref         0.0979
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7034
_reflns_number_total             8651
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03477k2.cif
_cod_data_source_block           zs-3
_cod_depositor_comments
'Adding full bibliography for 7705816--7705819.cif.'
_cod_database_code               7705816
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         DyCNO
_shelx_estimated_absorpt_t_max   0.782
_shelx_estimated_absorpt_t_min   0.672
_reflns_odcompleteness_completeness 98.65
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H48A,H48B,H48C} of C48, All C(H,H) groups
 At 1.5 times of:
  {H47A,H47B,H47C} of C47, {H49A,H49B,H49C} of C49, {H6A,H6B,H6C} of C6
2. Uiso/Uaniso restraints and constraints
O8 \\sim C49: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008
O9 \\sim O10 \\sim C50 \\sim C51 \\sim C52 \\sim C53: within 1.7A with sigma of
0.004 and sigma for terminal atoms of 0.008
3.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B), C19(H19A,H19B), C20(H20A,H20B), C23(H23A,
 H23B), C24(H24A,H24B), C50(H50A,H50B), C51(H51A,H51B), C52(H52A,H52B),
 C53(H53A,H53B)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C14(H14), C17(H17), C18(H18), C21(H21), C25(H25), C26(H26), C27(H27),
 C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C37(H37),
  C39(H39), C40(H40), C41(H41), C42(H42), C43(H43), C44(H44), C46(H46)
3.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C)
;
_shelx_res_checksum              2947
_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 1.586
_oxdiff_exptl_absorpt_empirical_full_min 0.675