Planar Dy3 + Dy3 clusters: design, structure and axial ligand perturbed magnetic dynamics.
Li, Xiao-Lei; Li, Han; Chen, Di-Ming; Wang, Chao; Wu, Jianfeng; Tang, Jinkui; Shi, Wei; Cheng, Peng; Dalton transactions (Cambridge, England : 2003) 44 (2015) 20316–20320; doi:10.1039/c5dt03931b

data_7037147
_publ_section_title
;
 Planar Dy3 + Dy3 clusters: design, structure and axial ligand perturbed
 magnetic dynamics.
;
_journal_issue                   47
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              20316
_journal_page_last               20320
_journal_paper_doi               10.1039/c5dt03931b
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety
'C24 H25 Dy3 N10 O9 S4, 0.5(C2 N), 2.75(C2 H3 N), 0.5(C H4 O), O'
_chemical_formula_sum            'C31 H35.25 Dy3 N13.25 O10.5 S4'
_chemical_formula_weight         1377.21
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-07-13
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-08-18 deposited with the CCDC.
2015-10-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 129.65(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   40.411(8)
_cell_length_b                   11.713(2)
_cell_length_c                   30.558(6)
_cell_measurement_reflns_used    10603
_cell_measurement_temperature    113.1500
_cell_measurement_theta_max      27.9223
_cell_measurement_theta_min      1.3483
_cell_volume                     11137(6)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution
;
????
;
_diffrn_ambient_temperature      113.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details
;
scan:
    Number of images: 90
               Slice: -120.0000 - 60.0000
         Image width: 2.0000
            Exp time: 2.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 0.0000
                 XTD: 60.2424
              2theta: -30.0069
scan:
    Number of images: 70
               Slice: -120.0000 - 20.0000
         Image width: 2.0000
            Exp time: 2.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 90.0000
                 XTD: 60.2424
              2theta: -30.0069
scan:
    Number of images: 60
               Slice: -120.0000 - 0.0000
         Image width: 2.0000
            Exp time: 2.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 180.0000
                 XTD: 60.2424
              2theta: -30.0069
;
_diffrn_measurement_device
;
Saturn70 (4x4 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       dtprofit.ref
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.0211
_diffrn_orient_matrix_UB_12      -0.0095
_diffrn_orient_matrix_UB_13      0.0223
_diffrn_orient_matrix_UB_21      0.0095
_diffrn_orient_matrix_UB_22      -0.0810
_diffrn_orient_matrix_UB_23      -0.0253
_diffrn_orient_matrix_UB_31      0.0066
_diffrn_orient_matrix_UB_32      -0.0118
_diffrn_orient_matrix_UB_33      0.0403
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0775
_diffrn_reflns_av_unetI/netI     0.0804
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            33379
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         1.309
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           16.0000
_diffrn_source_power             0.8000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    4.189
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4914
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.643
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             5280
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.604
_refine_diff_density_min         -1.602
_refine_diff_density_rms         0.222
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     637
_refine_ls_number_reflns         10824
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0955
_refine_ls_R_factor_gt           0.0741
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0693P)^2^+255.4697P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1806
_refine_ls_wR_factor_ref         0.1933
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8342
_reflns_number_total             10824
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03931b2.cif
_cod_data_source_block           r150126c
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 7037146--7037147.cif.
;
_cod_original_cell_volume        11137(5)
_cod_original_formula_sum        'C31 H35.25 Dy3 N13.25 O10.50 S4'
_cod_database_code               7037147
_diffrn_number_total             13682
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 S4A-N8
 2.8 with sigma of 0.02
 S4A-C22 = S4-C22
 1.78 with sigma of 0.02
 S4-N8
 2.8 with sigma of 0.02
 S4A-N8 = S1A-N10
 2.78 with sigma of 0.01
 S1A-C24
 1.7 with sigma of 0.05
 N10-S1A
 2.85 with sigma of 0.005
 O7-H7
 0.9 with sigma of 0.02
 H7-Dy1
 2.9 with sigma of 0.02
 H7-Dy3
 2.9 with sigma of 0.02
 H3-Dy2
 2.9 with sigma of 0.02
3. Rigid bond restraints
 S1, S1A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 S1, S1A, S1B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
S1 \\sim S1A \\sim S1B: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Uanis(S4) \\sim Ueq, Uanis(S4A) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(O13) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(S1) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O12) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(S4A)=1-FVAR(1)
 Sof(S4)=FVAR(1)
 Fixed Sof: C28(0.75) N12(0.75) C29(0.75) H29A(0.75) H29B(0.75) H29C(0.75)
 O10(0.5) H10(0.5) O13(0.25) S1(0.32377) S1A(0.34623) S1B(0.33) O11(0.25)
 O12(0.5) C25(0.5) H25A(0.5) H25B(0.5) H25C(0.5)
6.a Rotating group:
 O9(H9A,H9B), O8(H8A,H8B)
6.b Aromatic/amide H refined with riding coordinates:
 N2(H2), C8(H8), C3(H3A), C19(H19), C20(H20), C4(H4), C17(H17), C5(H5),
 C14(H14), C12(H12), C13(H13), N5(H5A)
6.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C31(H31A,H31B,H31C), C33(H33A,H33B,H33C), C10(H10A,H10B,
 H10C), C29(H29A,H29B,H29C), C25(H25A,H25B,H25C)
6.d Idealised tetrahedral OH refined as rotating group:
 O10(H10)
;
_shelx_res_checksum              44070
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'