Modulation of the relaxation dynamics of linear-shaped tetranuclear rare-earth clusters through utilizing different solvents.
Zhang, Ru-Xia; Chang, Yi-Xin; Shen, Hai-Yun; Wang, Wen-Min; Zhou, Xiao-Pu; Wang, Ni-Ni; Cui, Jian-Zhong; Gao, Hong-Ling; Dalton transactions (Cambridge, England : 2003) 45 (2016) 19117–19126; doi:10.1039/c6dt03500k

data_7041134
_publ_section_title
;
 Modulation of the relaxation dynamics of linear-shaped tetranuclear
 rare-earth clusters through utilizing different solvents.
;
_journal_issue                   47
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              19117
_journal_page_last               19126
_journal_paper_doi               10.1039/c6dt03500k
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C150 H120 Dy4 N8 O24, 3(C2 H3 N)'
_chemical_formula_sum            'C156 H129 Dy4 N11 O24'
_chemical_formula_weight         3191.69
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-06-17
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-11-04 deposited with the CCDC.
2016-11-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.768(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.720(2)
_cell_length_b                   18.621(2)
_cell_length_c                   24.284(3)
_cell_measurement_reflns_used    20209
_cell_measurement_temperature    113
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     7072.5(15)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)
;
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      113
_diffrn_detector                 PILT
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
scan:
    Number of images: 360
               Slice: -105.0000 - 75.0000
         Image width: 0.5000
            Exp time: 4.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 0.0000
                 XTD: 44.9263
              2theta: -15.0986
scan:
    Number of images: 300
               Slice: -105.0000 - 45.0000
         Image width: 0.5000
            Exp time: 4.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 90.0000
                 XTD: 44.9263
              2theta: -15.0986
scan:
    Number of images: 200
               Slice: -105.0000 - -5.0000
         Image width: 0.5000
            Exp time: 4.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 180.0000
                 XTD: 44.9263
              2theta: -15.0986
;
_diffrn_measurement_device
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Rigaku Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.000282
_diffrn_orient_matrix_UB_12      0.055488
_diffrn_orient_matrix_UB_13      -0.031759
_diffrn_orient_matrix_UB_21      0.032116
_diffrn_orient_matrix_UB_22      0.021257
_diffrn_orient_matrix_UB_23      0.037425
_diffrn_orient_matrix_UB_31      0.033022
_diffrn_orient_matrix_UB_32      -0.008750
_diffrn_orient_matrix_UB_33      -0.023367
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_unetI/netI     0.0201
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            71076
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.570
_diffrn_reflns_theta_min         3.022
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    2.162
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.824
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_density_method    "'not measured'"
_exptl_crystal_description       Prism
_exptl_crystal_F_000             3196
_exptl_crystal_preparation       Fiber
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.116
_refine_diff_density_min         -0.715
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     951
_refine_ls_number_reflns         16232
_refine_ls_number_restraints     52
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0281
_refine_ls_R_factor_gt           0.0220
_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^)+(0.0343P)^2^+5.7538P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0622
_refine_ls_wR_factor_ref         0.0648
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13856
_reflns_number_total             16232
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt03500k2.cif
_cod_data_source_block           8
_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 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7041127--7041135.cif.
;
_cod_original_cell_volume        7072.8(15)
_cod_database_code               7041134
_shelx_estimated_absorpt_t_max   0.781
_shelx_estimated_absorpt_t_min   0.672
_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, All O(H) groups, All O(H,H) groups
2. Restrained distances
 C74-C75 = C74'-C75'
 1.54 with sigma of 0.01
 O12-C74 = O12-C74'
 1.42 with sigma of 0.01
 O12-H12
 0.87 with sigma of 0.01
 O12-H12A
 0.87 with sigma of 0.01
 C74-H12
 1.925183 with sigma of 0.02
 Dy1-H12
 3.053834 with sigma of 0.02
 C74'-H12A
 1.896097 with sigma of 0.02
 Dy1-H12A
 2.9129 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N5) \\sim Ueq, Uanis(C76) \\sim Ueq, Uanis(C77) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.02
Uanis(C74) \\sim Ueq, Uanis(C75) \\sim Ueq, Uanis(C74') \\sim Ueq, Uanis(C75')
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(H12A)=Sof(C74')=Sof(H74C)=Sof(H74D)=Sof(C75')=Sof(H75D)=Sof(H75E)=
 Sof(H75F)=1-FVAR(1)
 Sof(H12)=Sof(C74)=Sof(H74A)=Sof(H74B)=Sof(C75)=Sof(H75A)=Sof(H75B)=Sof(H75C)=
 FVAR(1)
 Sof(C44A)=Sof(H44A)=Sof(C45A)=Sof(H45A)=Sof(C46A)=Sof(H46A)=Sof(C47A)=
 Sof(H47A)=Sof(C48A)=Sof(H48A)=Sof(C49A)=1-FVAR(2)
 Sof(C44)=Sof(H44)=Sof(C45)=Sof(H45)=Sof(C46)=Sof(H46)=Sof(C47)=Sof(H47)=
 Sof(C48)=Sof(H48)=Sof(C49)=FVAR(2)
 Fixed Sof: N5(0.5) C76(0.5) C77(0.5) H77A(0.5) H77B(0.5) H77C(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C74(H74A,H74B), C74'(H74C,H74D)
5.b Me refined with riding coordinates:
 C13(H13A,H13B,H13C), C75(H75A,H75B,H75C), C75'(H75D,H75E,H75F)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3A), C4(H4), C5(H5), C7(H7), C8(H8), C10(H10), C14(H14), C15(H15),
 C16(H16), C17(H17), C18(H18), C21(H21), C24(H24), C25(H25), C26(H26), C27(H27),
  C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33), C36(H36),
 C39(H39), C40(H40), C41(H41), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46),
  C47(H47), C48(H48), C51(H51), C54(H54), C55(H55), C56(H56), C57(H57),
 C58(H58), C59(H59), C60(H60), C61(H61), C62(H62), C63(H63), C66(H66), C69(H69),
  C70(H70), C71(H71), C72(H72), C73(H73), C44A(H44A), C45A(H45A), C46A(H46A),
 C47A(H47A), C48A(H48A)
5.d Fitted hexagon refined as free rotating group:
 C44(C45,C46,C47,C48,C49), C44A(C45A,C46A,C47A,C48A,C49A)
5.e Idealised Me refined as rotating group:
 C77(H77A,H77B,H77C), C79(H79A,H79B,H79C)
5.f Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_shelx_res_checksum              59015
_shelx_shelxl_version_number     2014/8
_olex2_submission_special_instructions 'No special instructions were received'