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_7041128
_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 N10 O24 Tb4, 2(C2 H3 N)'
_chemical_formula_sum            'C156 H128 N12 O24 Tb4'
_chemical_formula_weight         3190.43
_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                 99.887(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.342(2)
_cell_length_b                   27.548(4)
_cell_length_c                   19.000(3)
_cell_measurement_reflns_used    7746
_cell_measurement_temperature    113
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     7395.3(19)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
scan:
    Number of images: 360
               Slice: -105.0000 - 75.0000
         Image width: 0.5000
            Exp time: 8.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 0.0000
                 XTD: 44.9648
              2theta: -15.0719
scan:
    Number of images: 300
               Slice: -105.0000 - 45.0000
         Image width: 0.5000
            Exp time: 8.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 90.0000
                 XTD: 44.9648
              2theta: -15.0719
scan:
    Number of images: 200
               Slice: -105.0000 - -5.0000
         Image width: 0.5000
            Exp time: 8.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 180.0000
                 XTD: 44.9648
              2theta: -15.0719
;
_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      0.037130
_diffrn_orient_matrix_UB_12      -0.025794
_diffrn_orient_matrix_UB_13      0.054452
_diffrn_orient_matrix_UB_21      0.030902
_diffrn_orient_matrix_UB_22      0.008564
_diffrn_orient_matrix_UB_23      -0.017014
_diffrn_orient_matrix_UB_31      0.004250
_diffrn_orient_matrix_UB_32      0.044070
_diffrn_orient_matrix_UB_33      0.029901
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1193
_diffrn_reflns_av_unetI/netI     0.0898
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            61849
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.019
_diffrn_reflns_theta_max         25.019
_diffrn_reflns_theta_min         3.108
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.960
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.478
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_density_method    "'not measured'"
_exptl_crystal_description       Prism
_exptl_crystal_F_000             3200
_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         3.599
_refine_diff_density_min         -0.988
_refine_diff_density_rms         0.225
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     927
_refine_ls_number_reflns         12971
_refine_ls_number_restraints     115
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.1169
_refine_ls_R_factor_gt           0.0750
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0859P)^2^+81.9833P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1827
_refine_ls_wR_factor_ref         0.2143
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8882
_reflns_number_total             12971
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt03500k2.cif
_cod_data_source_block           2
_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        7395.4(18)
_cod_database_code               7041128
_shelx_estimated_absorpt_t_max   0.799
_shelx_estimated_absorpt_t_min   0.695
_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
 O12-C74 = O12-C74'
 1.24 with sigma of 0.01
 N5-C74 = N5-C75 = N5-C76 = N5'-C74' = N5'-C75' = N5'-C76'
 1.48 with sigma of 0.01
 C74-C75 \\sim C74-C76 \\sim C75-C76 \\sim C74'-C75' \\sim C74'-C76' \\sim
C75'-C76'
 with sigma of 0.01
3. Restrained planarity
 C74, C75, C76, N5
 with sigma of 0.01
 C74', C75', C76', N5'
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C44) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C47)
\\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C49) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C44') \\sim Ueq, Uanis(C45') \\sim Ueq, Uanis(C46') \\sim Ueq,
Uanis(C47') \\sim Ueq, Uanis(C48') \\sim Ueq, Uanis(C49') \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C75) \\sim Ueq, Uanis(C75') \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C74) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C74) = Uanis(C74')
Uanis(N5) = Uanis(N5')
Uanis(C76) = Uanis(C76')
Uanis(C44) = Uanis(C44')
Uanis(C45) = Uanis(C45')
5. Others
 Sof(C44')=Sof(H44')=Sof(C45')=Sof(H45')=Sof(C46')=Sof(H46')=Sof(C47')=
 Sof(H47')=Sof(C48')=Sof(H48')=Sof(C49')=Sof(C75')=Sof(H75D)=Sof(H75E)=
 Sof(H75F)=Sof(N5')=Sof(C74')=Sof(H74')=Sof(C76')=Sof(H76D)=Sof(H76E)=Sof(H76F)=
 1-FVAR(1)
 Sof(C44)=Sof(H44)=Sof(C45)=Sof(H45)=Sof(C46)=Sof(H46)=Sof(C47)=Sof(H47)=
 Sof(C48)=Sof(H48)=Sof(C49)=Sof(N5)=Sof(C74)=Sof(H74)=Sof(C76)=Sof(H76A)=
 Sof(H76B)=Sof(H76C)=Sof(C75)=Sof(H75A)=Sof(H75B)=Sof(H75C)=FVAR(1)
6.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), 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), C74(H74), C74'(H74')
6.b Fitted hexagon refined as free rotating group:
 C44(C45,C46,C47,C48,C49), C44'(C45',C46',C47',C48',C49')
6.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C80(H80A,H80B,H80C), C76(H76A,H76B,H76C), C75(H75A,H75B,
 H75C), C75'(H75D,H75E,H75F), C76'(H76D,H76E,H76F)
6.d Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_shelx_res_checksum              15861
_shelx_fab_checksum              12797
_shelx_shelxl_version_number     2014/8
_olex2_submission_special_instructions 'No special instructions were received'