Studies of Er(iii)‒W(v) compounds showing nonlinear optical activity and single-molecule magnetic properties
Kumar, Kunal; Stefanczyk, Olaf; Nakabayashi, Koji; Imoto, Kenta; Ohkoshi, Shin-ichi; CrystEngComm 21 (2019) 5882–; doi:10.1039/C9CE00822E

data_7233264
_publ_section_title
;
 Studies of Er(iii)--W(v) compounds showing nonlinear optical activity and
 single-molecule magnetic properties
;
_journal_issue                   39
_journal_name_full               CrystEngComm
_journal_page_first              5882
_journal_paper_doi               10.1039/C9CE00822E
_journal_volume                  21
_journal_year                    2019
_chemical_absolute_configuration rmad
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C28 H45 Er N13 O5 W'
_chemical_formula_sum            'C28 H45 Er N13 O5 W'
_chemical_formula_weight         994.88
_chemical_name_systematic
Pentakis(N,N-dimethylacetamide)erbium(III)octacyanidotungstate(V)
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-05-08T13:07:00-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2019-05-13 deposited with the CCDC.    2019-07-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.168(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.7633(4)
_cell_length_b                   19.5696(8)
_cell_length_c                   10.4110(5)
_cell_measurement_reflns_used    16082
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      3.04
_cell_volume                     1878.89(17)
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      89.95
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_unetI/netI     0.0629
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            17974
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.466
_diffrn_reflns_theta_min         3.035
_exptl_absorpt_coefficient_mu    5.329
_exptl_absorpt_correction_T_max  0.0905
_exptl_absorpt_correction_T_min  0.0149
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            'clear light pink'
_exptl_crystal_density_diffrn    1.759
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             972
_exptl_crystal_preparation
'Second Harmonic Generation,Magnetic properties'
_exptl_crystal_size_max          0.503
_exptl_crystal_size_mid          0.354
_exptl_crystal_size_min          0.088
_refine_diff_density_max         1.168
_refine_diff_density_min         -1.842
_refine_diff_density_rms         0.141
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.050(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     528
_refine_ls_number_reflns         8389
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.037
_refine_ls_R_factor_gt           0.0338
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0080P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0529
_refine_ls_wR_factor_ref         0.0536
_reflns_Friedel_coverage         0.943
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                8008
_reflns_number_total             8389
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce00822e2.cif
_cod_data_source_block           1_ErWdma5
_cod_depositor_comments
'Adding full bibliography for 7233262--7233264.cif.'
_cod_database_code               7233264
_shelx_estimated_absorpt_t_min   0.175
_shelx_estimated_absorpt_t_max   0.651
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.950(11)
 0.050(11)
2. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(O4) \\sim Ueq, Uanis(N12A) \\sim Ueq, Uanis(N12B) \\sim Ueq, Uanis(C9)
\\sim Ueq, Uanis(C13B) \\sim Ueq, Uanis(C15B) \\sim Ueq, Uanis(C21A) \\sim Ueq,
Uanis(C21B) \\sim Ueq, Uanis(C22B) \\sim Ueq, Uanis(C23B) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
4. Others
 Sof(H24D)=Sof(H24E)=Sof(H24F)=Sof(C23B)=Sof(H23A)=Sof(H23B)=Sof(H23C)=
 Sof(N12B)=Sof(C21B)=Sof(C22B)=Sof(H22D)=Sof(H22E)=Sof(H22F)=1-FVAR(1)
 Sof(H24A)=Sof(H24B)=Sof(H24C)=Sof(N12A)=Sof(C21A)=Sof(C23A)=Sof(H23D)=
 Sof(H23E)=Sof(H23F)=Sof(C22A)=Sof(H22A)=Sof(H22B)=Sof(H22C)=FVAR(1)
 Sof(C15B)=Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(C14B)=Sof(H14D)=Sof(H14E)=
 Sof(H14F)=Sof(C13B)=Sof(C16B)=Sof(H16D)=Sof(H16E)=Sof(H16F)=1-FVAR(2)
 Sof(C13A)=Sof(C15A)=Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(C16A)=Sof(H16A)=
 Sof(H16B)=Sof(H16C)=Sof(C14A)=Sof(H14A)=Sof(H14B)=Sof(H14C)=FVAR(2)
5.a Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C20(H20A,H20B,H20C), C10(H10A,H10B,H10C), C26(H26A,H26B,
 H26C), C19(H19A,H19B,H19C), C11(H11A,H11B,H11C), C18(H18A,H18B,H18C), C27(H27A,
 H27B,H27C), C24(H24A,H24B,H24C), C24(H24D,H24E,H24F), C28(H28A,H28B,H28C),
 C15A(H15A,H15B,H15C), C16A(H16A,H16B,H16C), C14A(H14A,H14B,H14C), C23B(H23A,
 H23B,H23C), C23A(H23D,H23E,H23F), C15B(H15D,H15E,H15F), C14B(H14D,H14E,H14F),
 C16B(H16D,H16E,H16F), C22A(H22A,H22B,H22C), C22B(H22D,H22E,H22F)
;
_olex2_submission_special_instructions 'No special instructions were received'