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_7705817
_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'
_chemical_formula_sum            'C49 H47 Dy N4 O8'
_chemical_formula_weight         982.40
_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     dual
_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                 115.130(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   31.8697(5)
_cell_length_b                   10.4652(2)
_cell_length_c                   32.2150(5)
_cell_measurement_reflns_used    12732
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      75.5930
_cell_measurement_theta_min      2.9680
_cell_volume                     9727.4(3)
_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 0.972
_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    -79.00  20.00   1.00    0.35    --  -48.45  94.00 -49.00   99
  2  \w    -14.00  12.00   1.00    0.35    --   48.45 -94.00-160.00   26
  3  \w     51.00  77.00   1.00    0.35    --   48.45 -94.00-160.00   26
  4  \w    -83.00 -15.00   1.00    1.70    --  -86.25  94.00 -49.00   68
  5  \w   -144.00-119.00   1.00    1.70    --  -86.25 -94.00-160.00   25
  6  \w     65.00 108.00   1.00    1.70    --  106.49 -94.00-160.00   43
  7  \w   -119.00 -70.00   1.00    0.35    --  -48.45-125.00   0.00   49
  8  \w    -63.00  12.00   1.00    0.35    --  -48.45  57.00-150.00   75
  9  \w    -99.00 -13.00   1.00    1.70    --  -86.25  19.00 -30.00   86
 10  \w     34.00 120.00   1.00    1.70    --  106.49 -57.00-180.00   86
 11  \w     84.00 178.00   1.00    1.70    --  106.49  77.00 -60.00   94
 12  \w     95.00 178.00   1.00    1.70    --  106.49  19.00  60.00   83
 13  \w    116.00 141.00   1.00    1.70    --  106.49  94.00 -49.00   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      -0.0323163000
_diffrn_orient_matrix_UB_12      -0.0359696000
_diffrn_orient_matrix_UB_13      0.0226854000
_diffrn_orient_matrix_UB_21      -0.0083284000
_diffrn_orient_matrix_UB_22      -0.1320200000
_diffrn_orient_matrix_UB_23      -0.0232976000
_diffrn_orient_matrix_UB_31      0.0416755000
_diffrn_orient_matrix_UB_32      -0.0540698000
_diffrn_orient_matrix_UB_33      0.0416466000
_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  0.0541
_diffrn_reflns_av_unetI/netI     0.0524
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            25906
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.079
_diffrn_reflns_theta_min         3.030
_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    8.657
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54548
_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    1.342
_exptl_crystal_description       block
_exptl_crystal_F_000             3992
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.435
_refine_diff_density_min         -0.700
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     563
_refine_ls_number_reflns         8564
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0585P)^2^+15.4329P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1035
_refine_ls_wR_factor_ref         0.1157
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7215
_reflns_number_total             8564
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03477k2.cif
_cod_data_source_block           zs1
_cod_depositor_comments
'Adding full bibliography for 7705816--7705819.cif.'
_cod_database_code               7705817
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         DyCNO
_shelx_estimated_absorpt_t_max   0.723
_shelx_estimated_absorpt_t_min   0.582
_reflns_odcompleteness_completeness 98.71
_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.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C13(H13A,H13B), C21(H21A,H21B), C24(H24A,H24B), C26(H26A,H26B),
 C39(H39A,H39B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C8(H8), C10(H10), C11(H11), C14(H14), C20(H20), C23(H23), C25(H25),
 C29(H29), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36),
  C37(H37), C38(H38), C41(H41), C42(H42), C43(H43), C44(H44), C46(H46)
2.c Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C49(H49A,H49B,
 H49C)
;
_shelx_res_checksum              42596
_shelx_fab_checksum              25953
_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 1.510
_oxdiff_exptl_absorpt_empirical_full_min 0.679