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_7233262
_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         'C20 H49 Er N5 O7, C8 N8 W, C4 H9 N O, H2 O'
_chemical_formula_sum            'C32 H60 Er N14 O9 W'
_chemical_formula_weight         1136.04
_chemical_name_systematic
'Di(aqua)Pentakis(N,N-dimethylacetamide)erbium(III)octacyanidotungstate(V) N,N-dimethylacetamide and aqua solvated'
_chemical_properties_physical    Moisture-sensitive,Moisture-sensitive
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-05-14T19:16:25-00:00
_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                 95.634(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.8904(2)
_cell_length_b                   22.5488(5)
_cell_length_c                   20.4885(4)
_cell_measurement_reflns_used    26015
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.02
_cell_volume                     4547.20(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_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0925
_diffrn_reflns_av_unetI/netI     0.08
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            41500
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.131
_exptl_absorpt_coefficient_mu    4.422
_exptl_absorpt_correction_T_max  0.1096
_exptl_absorpt_correction_T_min  0.0166
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_density_diffrn    1.659
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2256
_exptl_crystal_preparation       'Magnetic properties,Magnetic properties'
_exptl_crystal_size_max          0.418
_exptl_crystal_size_mid          0.167
_exptl_crystal_size_min          0.073
_refine_diff_density_max         2.104
_refine_diff_density_min         -2.436
_refine_diff_density_rms         0.205
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         10326
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_gt           0.0529
_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^)+(0.0291P)^2^+27.9536P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0975
_refine_ls_wR_factor_ref         0.105
_reflns_Friedel_coverage         0
_reflns_number_gt                8296
_reflns_number_total             10326
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce00822e2.cif
_cod_data_source_block           2_ErWdma5_3H2O_dma
_cod_depositor_comments
'Adding full bibliography for 7233262--7233264.cif.'
_cod_database_code               7233262
_shelx_estimated_absorpt_t_min   0.259
_shelx_estimated_absorpt_t_max   0.738
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 O3-H3A = O3-H3B
 0.87 with sigma of 0.02
 O1-H1A = O1-H1B
 0.87 with sigma of 0.02
 O8-H8A = O8-H8B
 0.87 with sigma of 0.02
 H3A-H3B
 1.38 with sigma of 0.04
 H1A-H1B
 1.38 with sigma of 0.04
 H8A-H8B
 1.38 with sigma of 0.04
 Er1-H3A \\sim Er1-H3B
 with sigma of 0.02
 Er1-H1A \\sim Er1-H1B
 with sigma of 0.02
3.a Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C12(H12A,H12B,H12C), C27(H27A,H27B,H27C), C22(H22A,H22B,
 H22C), C10(H10A,H10B,H10C), C32(H32A,H32B,H32C), C15(H15A,H15B,H15C), C18(H18A,
 H18B,H18C), C31(H31A,H31B,H31C), C19(H19A,H19B,H19C), C30(H30A,H30B,H30C),
 C14(H14A,H14B,H14C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C28(H28A,H28B,
 H28C), C11(H11A,H11B,H11C), C16(H16A,H16B,H16C), C20(H20A,H20B,H20C)
;
_olex2_submission_special_instructions 'No special instructions were received'