Asymmetry-unit-dominated double slow-relaxation modes of 2,6-dimethyl-3,5-heptanedione dysprosium SMMs
Shi, Chao; Nie, Rong; Yao, Xu; Fan, Siqi; An, Guanghui; Dong, Yanping; Li, Guangming; RSC Adv. 7 (2017) 49701–; doi:10.1039/C7RA09711E

data_7229404
_publ_section_title
;
 Asymmetry-unit-dominated double slow-relaxation modes of
 2,6-dimethyl-3,5-heptanedione dysprosium SMMs
;
_journal_issue                   78
_journal_name_full               'RSC Adv.'
_journal_page_first              49701
_journal_paper_doi               10.1039/C7RA09711E
_journal_volume                  7
_journal_year                    2017
_chemical_formula_moiety         'C37 H53 Lu N2 O6'
_chemical_formula_sum            'C37 H53 Lu N2 O6'
_chemical_formula_weight         796.27
_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   geom
_audit_creation_date             2017-07-19
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-07-19 deposited with the CCDC.
2017-10-12 downloaded from the CCDC.
;
_cell_angle_alpha                90.622(5)
_cell_angle_beta                 94.243(5)
_cell_angle_gamma                90.447(5)
_cell_formula_units_Z            4
_cell_length_a                   12.910(5)
_cell_length_b                   16.376(5)
_cell_length_c                   17.851(5)
_cell_measurement_reflns_used    14322
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.7728
_cell_measurement_theta_min      3.2193
_cell_volume                     3763(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  MoK\a
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0345
_diffrn_reflns_av_unetI/netI     0.0488
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            29384
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         3.226
_exptl_absorpt_coefficient_mu    2.667
_exptl_absorpt_correction_T_max  0.619
_exptl_absorpt_correction_T_min  0.533
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_description       block
_exptl_crystal_F_000             1630
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.481
_refine_diff_density_min         -1.355
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     853
_refine_ls_number_reflns         13241
_refine_ls_number_restraints     304
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0297
_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^)+(0.0170P)^2^+4.0882P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0616
_refine_ls_wR_factor_ref         0.0672
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11162
_reflns_number_total             13241
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ra09711e2.cif
_cod_data_source_block           123_CCDC3
_cod_depositor_comments
;

2018-02-15
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C74 H105 Lu2 N4 O12'
_cod_original_formula_weight         1592.55
_cod_original_formula_moiety         'C37 H52 Lu N2 O6, C37 H53 Lu N2 O6'
_cod_original_formula_units_Z            2
_cod_database_code               7229404
_shelx_shelxl_version_number     2016/6
_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
2. Rigid bond restraints
 C23, C29, C47, C50, C68, C74, C86, C90, C14
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C25, C38, C40, C64, C79, C81, C6, C8, C12
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C14, C90
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Uiso/Uaniso restraints and constraints
C23 \\sim C29 \\sim C47 \\sim C50 \\sim C68 \\sim C74 \\sim C86 \\sim C90 \\sim
C14: within 3.8A with sigma of 0.04 and sigma for terminal atoms of 0.08
C25 \\sim C38 \\sim C40 \\sim C64 \\sim C79 \\sim C81 \\sim C6 \\sim C8 \\sim
C12: within 3.8A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C11) \\sim Ueq, Uanis(C40) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C14) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4.a Ternary CH refined with riding coordinates:
 C37(H37), C38(H38), C41(H41), C42(H42), C46(H46), C47(H47), C49(H49),
 C69(H69), C90(H90), C92(H92), C95(H95)
4.b Aromatic/amide H refined with riding coordinates:
 C34(H34), C45(H45), C48(H48), C51(H51), C52(H52), C57(H57), C61(H61),
 C62(H62), C63(H63), C66(H66), C67(H67), C70(H70), C73(H73), C74(H74), C75(H75),
  C76(H76), C79(H79), C80(H80), C88(H88), C91(H91), C93(H93), C10(H10)
4.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C29(H29A,
 H29B,H29C), C50(H50A,H50B,H50C), C55(H55A,H55B,H55C), C85(H85A,H85B,H85C),
 C89(H89A,H89B,H89C), C99(H99A,H99B,H99C), C1(H1A,H1B,H1C), C2(H2A,H2B,H2C),
 C4(H4A,H4B,H4C), C11(H11A,H11B,H11C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C8(H8A,
 H8B,H8C), C9(H9A,H9B,H9C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,
 H14B,H14C)
;
_shelx_res_checksum              5440
_olex2_submission_special_instructions 'No special instructions were received'