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_7041129
_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         'C152 H122 Dy4 N10 O24'
_chemical_formula_sum            'C152 H122 Dy4 N10 O24'
_chemical_formula_weight         3122.59
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-09-29
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2016-11-04 deposited with the CCDC.
2016-11-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.990(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.5775(12)
_cell_length_b                   18.5073(15)
_cell_length_c                   27.600(2)
_cell_measurement_reflns_used    15606
_cell_measurement_temperature    113
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     6757.9(9)
_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 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
scan:
    Number of images: 360
               Slice: -105.0000 - 75.0000
         Image width: 0.5000
            Exp time: 5.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 0.0000
                 XTD: 44.9403
              2theta: -15.0968
scan:
    Number of images: 360
               Slice: -105.0000 - 75.0000
         Image width: 0.5000
            Exp time: 5.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 90.0000
                 XTD: 44.9403
              2theta: -15.0968
scan:
    Number of images: 360
               Slice: -105.0000 - 75.0000
         Image width: 0.5000
            Exp time: 5.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 180.0000
                 XTD: 44.9403
              2theta: -15.0968
;
_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      -0.042785
_diffrn_orient_matrix_UB_12      -0.057654
_diffrn_orient_matrix_UB_13      0.023635
_diffrn_orient_matrix_UB_21      -0.019151
_diffrn_orient_matrix_UB_22      0.030671
_diffrn_orient_matrix_UB_23      0.040151
_diffrn_orient_matrix_UB_31      -0.031698
_diffrn_orient_matrix_UB_32      0.004849
_diffrn_orient_matrix_UB_33      -0.018823
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_unetI/netI     0.0260
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            83687
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.534
_diffrn_reflns_theta_min         3.018
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    2.261
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.856
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_density_method    "'not measured'"
_exptl_crystal_description       Prism
_exptl_crystal_F_000             3120
_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         1.081
_refine_diff_density_min         -1.485
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     890
_refine_ls_number_reflns         15525
_refine_ls_number_restraints     260
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0334
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0309P)^2^+17.1302P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0744
_refine_ls_wR_factor_ref         0.0815
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12842
_reflns_number_total             15525
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt03500k2.cif
_cod_data_source_block           3
_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        6758.0(10)
_cod_database_code               7041129
_shelx_estimated_absorpt_t_max   0.773
_shelx_estimated_absorpt_t_min   0.661
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C67-C68 = C67-C68'
 1.52 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C68 \\sim C69 \\sim C70 \\sim C71 \\sim C72 \\sim C73 \\sim C68' \\sim C69'
\\sim C70' \\sim C71' \\sim C72' \\sim C73': within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C68) \\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(C70) \\sim Ueq, Uanis(C71)
\\sim Ueq, Uanis(C72) \\sim Ueq, Uanis(C73) \\sim Ueq, Uanis(C68') \\sim Ueq,
Uanis(C69') \\sim Ueq, Uanis(C70') \\sim Ueq, Uanis(C71') \\sim Ueq,
Uanis(C72') \\sim Ueq, Uanis(C73') \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Fixed Sof: C68(0.5) C69(0.5) H69(0.5) C70(0.5) H70(0.5) C71(0.5) H71(0.5)
 C72(0.5) H72(0.5) C73(0.5) H73(0.5) C68'(0.5) C69'(0.5) H69'(0.5) C70'(0.5)
 H70'(0.5) C71'(0.5) H71'(0.5) C72'(0.5) H72'(0.5) C73'(0.5) H73'(0.5)
5.a 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), C69'(H69'), C70'(H70'), C71'(H71'),
 C72'(H72'), C73'(H73'), C74(H74)
5.b Fitted hexagon refined as free rotating group:
 C68(C69,C70,C71,C72,C73), C68'(C69',C70',C71',C72',C73')
5.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C75(H75A,H75B,H75C), C76(H76A,H76B,H76C)
5.d Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_shelx_res_checksum              74701
_shelx_fab_checksum              15475
_shelx_shelxl_version_number     2014/8
_olex2_submission_special_instructions 'No special instructions were received'