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_7703922
_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 Cl3 Dy O3 P2, C4 H8 O'
_chemical_formula_sum            'C44 H46 Cl3 Dy O4 P2'
_chemical_formula_weight         969.60
_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                83.8200(10)
_cell_angle_beta                 73.2070(10)
_cell_angle_gamma                86.0800(10)
_cell_formula_units_Z            2
_cell_length_a                   11.1577(3)
_cell_length_b                   13.7559(4)
_cell_length_c                   14.4609(4)
_cell_measurement_reflns_used    9661
_cell_measurement_temperature    100
_cell_measurement_theta_max      70.070
_cell_measurement_theta_min      3.234
_cell_volume                     2110.90(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      100.02
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.984
_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  0.0373
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            39685
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.141
_diffrn_reflns_theta_min         3.206
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    12.258
_exptl_absorpt_correction_T_max  0.7533
_exptl_absorpt_correction_T_min  0.3883
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1094 before and 0.0552 after correction. The Ratio of minimum to maximum transmission is 0.5155. 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    1.525
_exptl_crystal_description       block
_exptl_crystal_F_000             978
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.576
_refine_diff_density_min         -0.979
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     475
_refine_ls_number_reflns         7909
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0240
_refine_ls_R_factor_gt           0.0232
_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^)+(0.0287P)^2^+1.9351P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0588
_refine_ls_wR_factor_ref         0.0600
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7747
_reflns_number_total             7909
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00801j3.cif
_cod_data_source_block           vig136_dycl3
_cod_depositor_comments
'Adding full bibliography for 7703921--7703923.cif.'
_cod_database_code               7703922
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.321
_shelx_estimated_absorpt_t_min   0.193
_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(C8) = Uanis(C13) = Uanis(C9)
Uanis(C8) = Uanis(C9)
3.a Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C44(H44A,H44B), C22(H22A,H22B), C45(H45A,H45B), C43(H43A,
 H43B), C21(H21A,H21B), C20(H20A,H20B), C42(H42A,H42B)
3.b Aromatic/amide H refined with riding coordinates:
 C25(H25), C19(H19), C15(H15), C13(H13), C6(H6), C2(H2), C4(H4), C17(H17),
 C9(H9), C16(H16), C27(H27), C35(H35), C28(H28), C5(H5), C31(H31), C29(H29),
 C41(H41), C26(H26), C18(H18), C33(H33), C3(H3), C32(H32), C34(H34), C11(H11),
 C10(H10), C40(H40), C37(H37), C39(H39), C12(H12), C38(H38)
;
_shelx_res_checksum              86571
_olex2_submission_special_instructions 'No special instructions were received'