Magnetization dynamics of a heterometallic Dy-isocarbonyl complex
Dickie, Courtney M.; Nippe, Michael; Inorganic Chemistry Frontiers 3 (2016) 97–; doi:10.1039/C5QI00224A

data_4349035
_publ_section_title
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 Magnetization dynamics of a heterometallic Dy-isocarbonyl complex
;
_journal_issue                   1
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              97
_journal_paper_doi               10.1039/C5QI00224A
_journal_volume                  3
_journal_year                    2016
_chemical_formula_moiety         'C44 H55 Dy O14 W3, C4 H8 O'
_chemical_formula_sum            'C48 H63 Dy O15 W3'
_chemical_formula_weight         1594.03
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-10-19
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-10-19 deposited with the CCDC.
2015-12-04 downloaded from the CCDC.
;
_cell_angle_alpha                97.367(4)
_cell_angle_beta                 101.318(4)
_cell_angle_gamma                92.721(4)
_cell_formula_units_Z            2
_cell_length_a                   11.1292(8)
_cell_length_b                   11.2334(8)
_cell_length_c                   20.7030(16)
_cell_measurement_reflns_used    9927
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      25.2033
_cell_measurement_theta_min      2.2156
_cell_volume                     2509.9(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_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  0.0997
_diffrn_reflns_av_unetI/netI     0.0685
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            91582
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.487
_diffrn_reflns_theta_min         1.013
_exptl_absorpt_coefficient_mu    8.389
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5282
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.109
_exptl_crystal_description       block
_exptl_crystal_F_000             1518
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.413
_refine_diff_density_min         -1.772
_refine_diff_density_rms         0.262
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     595
_refine_ls_number_reflns         12574
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0431
_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^)+(0.0405P)^2^+6.7156P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0890
_refine_ls_wR_factor_ref         0.1027
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9102
_reflns_number_total             12574
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5qi00224a2.cif
_cod_data_source_block           'data_0m'
_cod_database_code               4349035
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.366
_shelx_estimated_absorpt_t_min   0.366
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C23) = Uanis(C22) = Uanis(C21) = Uanis(C20) = Uanis(C24)
3. Others
 Fixed Sof: H21(0.64) H21A(0.36) H22(0.64) H22A(0.36) C20(0.64) H20(0.64)
 C23(0.64) H23(0.64) C24(0.64) H24(0.64) C22A(0.36) H22B(0.36) C23A(0.36)
 H23A(0.36) C24A(0.36) H24A(0.36)
4.a Ternary CH refined with riding coordinates:
 C21(H21), C21(H21A), C22(H22), C22(H22A)
4.b Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,
 H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B),
 C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B),
  C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B), C43(H43A,
 H43B), C44(H44A,H44B), C1S(H1SA,H1SB), C2S(H2SA,H2SB), C3S(H3SA,H3SB),
 C4S(H4SA,H4SB)
4.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C17(H17),
 C18(H18), C19(H19), C20(H20), C23(H23), C24(H24), C22A(H22B), C23A(H23A),
 C24A(H24A)
;
_shelx_res_checksum              45353
_shelx_hkl_checksum              38735
_olex2_submission_special_instructions 'No special instructions were received'