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_7233263
_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 'synthesis as described'
_chemical_formula_moiety         'C28 H51.50 Er N13 O11 W'
_chemical_formula_sum            'C28 H51.5 Er N13 O11 W'
_chemical_formula_weight         1097.43
_chemical_name_systematic
'Tris(aqua)Tetrakis(N,N-dimethylacetamide)erbium(III)octacyanidotungstate(V) N,N-dimethylacetamide and aqua solvated'
_chemical_properties_physical    Moisture-sensitive
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-05-08T16:00:24-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2019-05-28 deposited with the CCDC.    2019-07-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.033(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.6140(8)
_cell_length_b                   18.1609(12)
_cell_length_c                   25.5697(18)
_cell_measurement_reflns_used    20613
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      3.06
_cell_volume                     4420.6(6)
_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      90(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_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  0.0987
_diffrn_reflns_av_unetI/netI     0.0859
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            42014
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         3.064
_exptl_absorpt_coefficient_mu    4.548
_exptl_absorpt_correction_T_max  0
_exptl_absorpt_correction_T_min  0
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            'clear green'
_exptl_crystal_density_diffrn    1.649
_exptl_crystal_description       needle
_exptl_crystal_F_000             2162
_exptl_crystal_preparation       'Magnetic properties,Magnetic properties'
_exptl_crystal_size_max          0.409
_exptl_crystal_size_mid          0.209
_exptl_crystal_size_min          0.147
_refine_diff_density_max         1.269
_refine_diff_density_min         -1.55
_refine_diff_density_rms         0.176
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     570
_refine_ls_number_reflns         10110
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0924
_refine_ls_R_factor_gt           0.0498
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0482P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0899
_refine_ls_wR_factor_ref         0.1013
_reflns_Friedel_coverage         0
_reflns_number_gt                7023
_reflns_number_total             10110
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce00822e2.cif
_cod_data_source_block           3_ErWdma5_6H2O
_cod_depositor_comments
'Adding full bibliography for 7233262--7233264.cif.'
_cod_original_formula_sum        'C28 H51.50 Er N13 O11 W'
_cod_database_code               7233263
_shelx_estimated_absorpt_t_min   0.258
_shelx_estimated_absorpt_t_max   0.554
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
: with sigma of 0.001 and sigma for terminal atoms of 0.002
: with sigma of 0.001 and sigma for terminal atoms of 0.002
: with sigma of 0.001 and sigma for terminal atoms of 0.002
3. Others
 Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(N10A)=Sof(H14D)=Sof(H14E)=Sof(H14F)=
 Sof(H16D)=Sof(H16E)=Sof(H16F)=Sof(C13)=1-FVAR(1)
 Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(H16A)=
 Sof(H16B)=Sof(H16C)=Sof(N10B)=Sof(C6B)=FVAR(1)
 Sof(H12D)=Sof(H12E)=Sof(H12F)=Sof(C10B)=Sof(H10A)=Sof(H10B)=Sof(H10C)=
 Sof(C11B)=Sof(H11A)=Sof(H11B)=Sof(H11C)=Sof(C9B)=Sof(N9B)=1-FVAR(2)
 Sof(N9A)=Sof(C9A)=Sof(H12A)=Sof(H12B)=Sof(H12C)=Sof(C11A)=Sof(H11D)=Sof(H11E)=
 Sof(H11F)=Sof(C10A)=Sof(H10D)=Sof(H10E)=Sof(H10F)=FVAR(2)
 Fixed Sof: O11A(0.5) C28(0.5) H28A(0.5) H28B(0.5) H28C(0.5) N13(0.5) C27(0.5)
 H27A(0.5) H27B(0.5) H27C(0.5) O10(0.5) C26(0.5) H26A(0.5) H26B(0.5) H26C(0.5)
 O11B(0.5) H11G(0.5) H11H(0.5) C32(0.66667) C30(0.33333) C31(0.5) O12(0.5)
 C25(0.5) C29(0.25) N14A(0.25) C25B(0.25) N14B(0.25)
4.a Fixed occupancy and ADP/Uiso:
 O1, O3, O4
4.b Free rotating group:
 O9(H9A,H9B), O8(H8A,H8B), O11B(H11G,H11H)
4.c Rotating group:
 O1(H1A,H1B), O3(H3A,H3B), O4(H4A,H4B)
4.d Idealised Me refined as rotating group:
 C15(H15D,H15E,H15F), C15(H15A,H15B,H15C), C14(H14D,H14E,H14F), C14(H14A,H14B,
 H14C), C16(H16D,H16E,H16F), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C19(H19A,
 H19B,H19C), C24(H24A,H24B,H24C), C12(H12A,H12B,H12C), C12(H12D,H12E,H12F),
 C23(H23A,H23B,H23C), C20(H20A,H20B,H20C), C10B(H10A,H10B,H10C), C22(H22A,H22B,
 H22C), C28(H28A,H28B,H28C), C27(H27A,H27B,H27C), C11B(H11A,H11B,H11C),
 C11A(H11D,H11E,H11F), C10A(H10D,H10E,H10F), C26(H26A,H26B,H26C)
;
_olex2_submission_special_instructions 'No special instructions were received'