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_7037146
_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         'C44 H54 Dy6 N14 O38, 10(O), 2(N O3)'
_chemical_formula_sum            'C44 H54 Dy6 N16 O54'
_chemical_formula_weight         2646.03
_chemical_name_systematic        lixl-Dy6-NO3
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-05-26
_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                100.954(2)
_cell_angle_beta                 100.243(2)
_cell_angle_gamma                109.293(2)
_cell_formula_units_Z            1
_cell_length_a                   10.7890(11)
_cell_length_b                   12.7071(13)
_cell_length_c                   16.9727(18)
_cell_measurement_reflns_used    5464
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      26.09
_cell_measurement_theta_min      2.43
_cell_volume                     2082.3(4)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        SAINT
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_av_unetI/netI     0.0567
_diffrn_reflns_laue_measured_fraction_full 0.948
_diffrn_reflns_laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11482
_diffrn_reflns_point_group_measured_fraction_full 0.948
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.762
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    5.427
_exptl_absorpt_correction_T_max  0.581
_exptl_absorpt_correction_T_min  0.283
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   (sadabs;bruker,2000)
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.110
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1258
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.984
_refine_diff_density_min         -1.509
_refine_diff_density_rms         0.217
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     558
_refine_ls_number_reflns         6956
_refine_ls_number_restraints     73
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0457
_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^)+(0.0765P)^2^+8.7372P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1271
_refine_ls_wR_factor_ref         0.1393
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5452
_reflns_number_total             6956
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03931b2.cif
_cod_data_source_block           lixl-Dy6-NO3
_cod_depositor_comments
'Adding full bibliography for 7037146--7037147.cif.'
_cod_database_code               7037146
_shelx_estimated_absorpt_t_max   0.613
_shelx_estimated_absorpt_t_min   0.293
_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,H) groups
2. Restrained distances
 H7-O7
 0.9 with sigma of 0.02
 H7-Dy3
 2.9 with sigma of 0.02
 H7-Dy2
 2.9 with sigma of 0.02
 H3-Dy2
 2.9 with sigma of 0.02
 H3-O3
 0.9 with sigma of 0.02
 O14-O15 \\sim O15-O16
 with sigma of 0.01
 O15-N6 \\sim O16-N6 \\sim O14-N6
 with sigma of 0.01
 O22-O20 \\sim O20-O21
 with sigma of 0.02
 O20-O21 \\sim O20-O22 \\sim O22-O21
 with sigma of 0.01
3. Rigid bond restraints
 O14, O15, O16, N6
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 O20, O21, O22, N8
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
O20 \\sim O21 \\sim O22 \\sim N8: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
O14 \\sim O15 \\sim O16 \\sim N6: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
Uanis(O26) \\sim Ueq, Uanis(O27) \\sim Ueq, Uanis(O27) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
5.a Rotating group:
 O8(H8A,H8B), O9(H9A,H9B), O10(H10A,H10B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3A), C4(H4), C5(H5), C8(H8), C9(H9), C11(H11), C12(H12), C14(H14),
 C15(H15), C17(H17), C18(H18), C19(H19)
5.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C22(H22A,H22B,H22C)
;
_shelx_res_checksum              39088
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'