Six-coordinate mononuclear dysprosium(iii) single-molecule magnets with the triphenylphosphine oxide ligand.
Vignesh, Kuduva R.; Alexandropoulos, Dimitris I.; Xie, Haomiao; Dunbar, Kim R.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 4694–4698; doi:10.1039/d0dt00801j

data_7703921
_publ_section_title
;
 Six-coordinate mononuclear dysprosium(iii) single-molecule magnets with
 the triphenylphosphine oxide ligand.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4694
_journal_page_last               4698
_journal_paper_doi               10.1039/d0dt00801j
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C40 H38 Br3 Dy O3 P2, C4 H8 O'
_chemical_formula_sum            'C44 H46 Br3 Dy O4 P2'
_chemical_formula_weight         1102.98
_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   geom
_audit_creation_date             2019-02-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-03-11 deposited with the CCDC.	2020-03-13 downloaded from the CCDC.
;
_cell_angle_alpha                82.8930(10)
_cell_angle_beta                 72.5020(10)
_cell_angle_gamma                85.9810(10)
_cell_formula_units_Z            2
_cell_length_a                   11.3337(3)
_cell_length_b                   14.1733(3)
_cell_length_c                   14.5035(4)
_cell_measurement_reflns_used    9801
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.126
_cell_measurement_theta_min      3.144
_cell_volume                     2203.57(10)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'APEX3 Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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      100.0
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0334
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            35611
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.118
_diffrn_reflns_theta_min         3.144
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    13.257
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.5181
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1215 before and 0.0502 after correction. The Ratio of minimum to maximum transmission is 0.6875. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.662
_exptl_crystal_description       block
_exptl_crystal_F_000             1086
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.382
_refine_diff_density_min         -0.689
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         8556
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0226
_refine_ls_R_factor_gt           0.0207
_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^)+(0.0165P)^2^+1.7164P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0472
_refine_ls_wR_factor_ref         0.0487
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8218
_reflns_number_total             8556
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00801j3.cif
_cod_data_source_block           vig148_dybr3
_cod_depositor_comments
'Adding full bibliography for 7703921--7703923.cif.'
_cod_original_cell_volume        2203.58(10)
_cod_database_code               7703921
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.351
_shelx_estimated_absorpt_t_min   0.241
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C40(H40A,H40B), C39(H39A,H39B), C38(H38A,H38B), C41(H41A,H41B), C37(H37A,
 H37B), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B)
2.b Aromatic/amide H refined with riding coordinates:
 C29(H29), C24(H24), C2(H2), C22(H22), C23(H23), C36(H36), C35(H35), C20(H20),
 C18(H18), C25(H25), C26(H26), C32(H32), C21(H21), C28(H28), C27(H27), C6(H6),
 C14(H14), C12(H12), C15(H15), C4(H4), C33(H33), C17(H17), C3(H3), C8(H8),
 C11(H11), C34(H34), C16(H16), C10(H10), C5(H5), C9(H9)
;
_shelx_res_checksum              48510
_olex2_submission_special_instructions 'No special instructions were received'