A method for extending AC susceptometry to long-timescale magnetic relaxation.
Hilgar, Jeremy D.; Butts, Aaron K.; Rinehart, Jeffrey D.; Physical chemistry chemical physics : PCCP  (2019) –; doi:10.1039/c9cp03936h

data_7234678
_publ_section_title
;
 A method for extending AC susceptometry to long-timescale magnetic
 relaxation.
;
_journal_name_full               'Physical chemistry chemical physics : PCCP'
_journal_paper_doi               10.1039/c9cp03936h
_journal_year                    2019
_chemical_formula_moiety         'C40 H56 Er K O6, 2(C4 H8 O)'
_chemical_formula_sum            'C48 H72 Er K O8'
_chemical_formula_weight         983.41
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_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
_audit_creation_date             2019-07-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-07-10 deposited with the CCDC.    2019-10-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.578(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.8556(5)
_cell_length_b                   20.0974(11)
_cell_length_c                   22.9588(12)
_cell_measurement_reflns_used    9908
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      54.02
_cell_measurement_theta_min      2.54
_cell_volume                     4542.9(4)
_computing_cell_refinement       '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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0677
_diffrn_reflns_av_unetI/netI     0.0535
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            34075
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         53.997
_diffrn_reflns_theta_min         2.543
_exptl_absorpt_coefficient_mu    6.864
_exptl_absorpt_correction_T_max  0.3012
_exptl_absorpt_correction_T_min  0.1857
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0884 before and 0.0618 after correction. The Ratio of minimum to maximum transmission is 0.6165. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_description       block
_exptl_crystal_F_000             2044
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Pentane vapor diffusion into THF solution.'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.347
_refine_diff_density_min         -1.072
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     548
_refine_ls_number_reflns         8303
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0422
_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^)+(0.0368P)^2^+7.5139P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0953
_refine_ls_wR_factor_ref         0.0996
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6926
_reflns_number_total             8303
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cp03936h2.cif
_cod_data_source_block           jr_386
_cod_database_code               7234678
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.684
_shelx_estimated_absorpt_t_min   0.547
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C48B-C47B \\sim C47A-C48A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C48A) = Uanis(C48B)
Uanis(C47B) = Uanis(C47A)
Uanis(O8A) = Uanis(O8B)
Uanis(C46A) = Uanis(C46B)
Uanis(C45A) = Uanis(C45B)
Uanis(O7A) = Uanis(O7B)
Uanis(C44A) = Uanis(C44B)
Uanis(C43A) = Uanis(C43B)
4. Others
 Sof(O7B)=Sof(O8B)=Sof(C43B)=Sof(H43A)=Sof(H43B)=Sof(C44B)=Sof(H44A)=Sof(H44B)=
 Sof(C45B)=Sof(H45A)=Sof(H45B)=Sof(C46B)=Sof(H46A)=Sof(H46B)=Sof(C47B)=
 Sof(H47A)=Sof(H47B)=Sof(C48B)=Sof(H48A)=Sof(H48B)=1-FVAR(1)
 Sof(O7A)=Sof(O8A)=Sof(C43A)=Sof(H43C)=Sof(H43D)=Sof(C44A)=Sof(H44C)=Sof(H44D)=
 Sof(C45A)=Sof(H45C)=Sof(H45D)=Sof(C46A)=Sof(H46C)=Sof(H46D)=Sof(C47A)=
 Sof(H47C)=Sof(H47D)=Sof(C48A)=Sof(H48C)=Sof(H48D)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,
 H27B), C28(H28A,H28B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B),
 C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B), C43B(H43A,H43B), C44B(H44A,
 H44B), C45B(H45A,H45B), C46B(H46A,H46B), C47B(H47A,H47B), C48B(H48A,H48B),
 C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B),
  C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C9(H9A,H9B), C10(H10A,H10B),
 C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C43A(H43C,
 H43D), C44A(H44C,H44D), C45A(H45C,H45D), C46A(H46C,H46D), C47A(H47C,H47D),
 C48A(H48C,H48D)
5.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C16(H16), C19(H19), C20(H20), C1(H1), C2(H2), C5(H5), C6(H6)
;
_shelx_res_checksum              64448
_shelx_hkl_checksum              19537
_olex2_submission_special_instructions 'No special instructions were received'