Slow magnetic relaxation in a homo dinuclear Dy(iii) complex in a pentagonal bipyramidal geometry.
Acharya, Joydev; Ahmed, Naushad; Flores Gonzalez, Jessica; Kumar, Pawan; Cador, Olivier; Singh, Saurabh Kumar; Pointillart, Fabrice; Chandrasekhar, Vadapalli; Dalton transactions (Cambridge, England : 2003) 49 (2020) 13110–13122; doi:10.1039/d0dt02881a

data_7705402
_publ_section_title
;
 Slow magnetic relaxation in a homo dinuclear Dy(iii) complex in a
 pentagonal bipyramidal geometry.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13110
_journal_page_last               13122
_journal_paper_doi               10.1039/d0dt02881a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C20 H18 Cl4 N6 O8 Y2, 2(C4 H10 O), O'
_chemical_formula_sum            'C28 H38 Cl4 N6 O11 Y2'
_chemical_formula_weight         954.26
_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             2020-05-19
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-05-20 deposited with the CCDC.	2020-09-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.379(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.9090(6)
_cell_length_b                   11.5451(6)
_cell_length_c                   22.9371(9)
_cell_measurement_reflns_used    7750
_cell_measurement_temperature    119.98(10)
_cell_measurement_theta_max      28.5790
_cell_measurement_theta_min      2.8560
_cell_volume                     3948.0(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      119.98(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.881
_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     -7.00  24.00   0.50   88.00    --   -7.60  21.00-105.00   62
  2  \w    -86.00 -60.00   0.50   88.00    --   -7.60  21.00-105.00   52
  3  \w    -77.00 -51.00   0.50   88.00    --    7.20  21.00-105.00   52
  4  \w     63.00  88.00   0.50   88.00    --    7.20  77.00 -30.00   50
  5  \w     50.00  75.00   0.50   88.00    --    7.20  77.00  30.00   50
  6  \w     54.00  95.00   0.50   88.00    --    7.20  77.00 120.00   82
  7  \w      0.00  86.00   0.50   88.00    --    7.20  57.00 -90.00  172
  8  \w    -62.00 -17.00   0.50   88.00    --   -7.60 -82.00-180.00   90
  9  \w    -44.00  30.00   0.50   88.00    --   -7.60 -82.00-120.00  148
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0425687000
_diffrn_orient_matrix_UB_12      0.0167322000
_diffrn_orient_matrix_UB_13      -0.0107842000
_diffrn_orient_matrix_UB_21      -0.0170089000
_diffrn_orient_matrix_UB_22      -0.0024752000
_diffrn_orient_matrix_UB_23      -0.0289310000
_diffrn_orient_matrix_UB_31      -0.0126563000
_diffrn_orient_matrix_UB_32      0.0590772000
_diffrn_orient_matrix_UB_33      0.0018137000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_unetI/netI     0.0388
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.881
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            20504
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.881
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.010
_diffrn_reflns_theta_min         2.732
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.256
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75431
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_description       block
_exptl_crystal_F_000             1928
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.429
_refine_diff_density_min         -1.024
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         4636
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0714
_refine_ls_R_factor_gt           0.0580
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0624P)^2^+41.3170P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1510
_refine_ls_wR_factor_ref         0.1561
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3855
_reflns_number_total             4636
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02881a2.cif
_cod_data_source_block           complex2
_cod_depositor_comments
'Adding full bibliography for 7705401--7705402.cif.'
_cod_database_code               7705402
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O Y Cl'
_shelx_estimated_absorpt_t_max   0.938
_shelx_estimated_absorpt_t_min   0.938
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.05
Uanis(O2) \\sim Ueq, Uanis(O2) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.005
3.a Secondary CH2 refined with riding coordinates:
 C00N(H00K,H00L), C1(H1A,H1B)
3.b Aromatic/amide H refined with riding coordinates:
 N009(H009), C00B(H00B), C00G(H00G), C00I(H00I), C00J(H00J)
3.c Idealised Me refined as rotating group:
 C00L(H00A,H00C,H00D), C00M(H00E,H00F,H00H), C0AA(H0AA,H0AB,H0AC)
3.d Idealised tetrahedral OH refined as rotating group:
 O007(H007)
;
_shelx_res_checksum              46492
_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 1.347
_oxdiff_exptl_absorpt_empirical_full_min 0.729