Synergistic effect of mixed ligands on the anisotropy axis of two dinuclear dysprosium complexes.
Ke, Hongshan; Yang, Yongsheng; Wei, Wen; Jiang, Youdong; Zhang, Yi-Quan; Xie, Gang; Chen, Sanping; Dalton transactions (Cambridge, England : 2003) 49 (2020) 10594–10602; doi:10.1039/d0dt02139c

data_7704900
_publ_section_title
;
 Synergistic effect of mixed ligands on the anisotropy axis of two
 dinuclear dysprosium complexes.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10594
_journal_page_last               10602
_journal_paper_doi               10.1039/d0dt02139c
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C82 H98 Dy2 N4 O14, 1.5(C H4 O)'
_chemical_formula_sum            'C83.5 H104 Dy2 N4 O15.5'
_chemical_formula_weight         1736.70
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-11-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-05-13 deposited with the CCDC.	2020-07-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   40.7539(19)
_cell_length_b                   40.7539(19)
_cell_length_c                   20.1854(9)
_cell_measurement_reflns_used    9958
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      25.466
_cell_measurement_theta_min      2.293
_cell_volume                     33526(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0834
_diffrn_reflns_av_unetI/netI     0.0528
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       -49
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            121120
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.710
_diffrn_reflns_theta_min         2.235
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.833
_exptl_absorpt_correction_T_max  0.2594
_exptl_absorpt_correction_T_min  0.2176
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0700 before and 0.0584 after correction. The Ratio of minimum to maximum transmission is 0.8389. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            Yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_description       plate
_exptl_crystal_F_000             14224
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.176
_refine_diff_density_min         -1.322
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1045
_refine_ls_number_reflns         15945
_refine_ls_number_restraints     88
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0872
_refine_ls_R_factor_gt           0.0505
_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^)+(0.0278P)^2^+330.0530P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1004
_refine_ls_wR_factor_ref         0.1163
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11138
_reflns_number_total             15945
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02139c2.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_colour_primary' value 'Yellow' was changed
to 'yellow' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7704900--7704901.cif.

 Adding full bibliography for 7704900--7704901.cif.
;
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_original_formula_sum        'C83.50 H104 Dy2 N4 O15.50'
_cod_database_code               7704900
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.838
_shelx_estimated_absorpt_t_min   0.810
_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 C(H,H,H,H,H,H) groups, All O(H) groups
2. Restrained distances
 O13-H13A
 0.87 with sigma of 0.01
 O14-H14
 0.87 with sigma of 0.01
 C81-H13A
 1.90048 with sigma of 0.02
 Dy2-H13A
 3.061865 with sigma of 0.02
 C82-H14
 1.890791 with sigma of 0.02
 Dy1-H14
 3.044039 with sigma of 0.02
 C33-C34 \\sim C33-C34A
 with sigma of 0.02
 C33-C35 \\sim C33-C35A
 with sigma of 0.02
 C33-C36 \\sim C33-C36A
 with sigma of 0.02
 O3AA-C1AA \\sim O0AA-C3AA
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C1AA \\sim O0AA \\sim O3AA \\sim C3AA: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C33, C34, C35, C36
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C33, C34, C34A, C36A, C35A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C1AA, O3AA
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 O0AA, C3AA
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
5. Others
 Sof(H0AD)=Sof(H0AE)=Sof(H0AF)=Sof(O1AA)=Sof(H1AA)=1-FVAR(1)
 Sof(C1AA)=Sof(H1AB)=Sof(H1AC)=Sof(H1AD)=Sof(O3AA)=Sof(H3AD)=0.5*(1-FVAR(2))
 Sof(O0AA)=Sof(H0AG)=Sof(C3AA)=Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=0.5*FVAR(2)
 Sof(H0AA)=Sof(H0AB)=Sof(H0AC)=Sof(O2AA)=Sof(H2AA)=FVAR(1)
 Sof(C34A)=Sof(H34D)=Sof(H34E)=Sof(H34F)=Sof(C36A)=Sof(H36D)=Sof(H36E)=
 Sof(H36F)=Sof(C35A)=Sof(H35D)=Sof(H35E)=Sof(H35F)=1-FVAR(2)
 Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=
 Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=FVAR(2)
6.a Riding coordinates:
 C0AA(H0AD,H0AE,H0AF), C0AA(H0AA,H0AB,H0AC), C3AA(H3AA,H3AB,H3AC)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C9(H9), C10(H10), C13(H13), C22(H22), C23(H23),
 C24(H24), C27(H27), C30(H30), C31(H31), C40(H40), C41(H41), C42(H42), C44(H44),
  C45(H45), C53(H53), C62(H62), C63(H63), C64(H64), C66(H66), C67(H67), C75(H75)
6.c Tetrahedral OH refined with riding coordinates:
 O1AA(H1AA), O2AA(H2AA), O0AA(H0AG), O3AA(H3AD)
6.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C), C19(H19A,H19B,H19C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,
 H36B,H36C), C37(H37A,H37B,H37C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C),
 C52(H52A,H52B,H52C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C58(H58A,H58B,
 H58C), C59(H59A,H59B,H59C), C72(H72A,H72B,H72C), C73(H73A,H73B,H73C), C74(H74A,
 H74B,H74C), C78(H78A,H78B,H78C), C79(H79A,H79B,H79C), C80(H80A,H80B,H80C),
 C81(H81A,H81B,H81C), C82(H82A,H82B,H82C), C34A(H34D,H34E,H34F), C36A(H36D,H36E,
 H36F), C35A(H35D,H35E,H35F), C1AA(H1AB,H1AC,H1AD)
;
_shelx_res_checksum              41228
_shelx_fab_checksum              54277
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'