Synthesis, Crystal Structures, Magnetic Properties, and Theoretical Investigation of a New Series of Ni<sup>II</sup>-Ln<sup>III</sup>-W<sup>V</sup> Heterotrimetallics: Understanding the SMM Behavior of Mixed Polynuclear Complexes.
Vieru, Veacheslav; Pasatoiu, Traian D.; Ungur, Liviu; Suturina, Elizaveta; Madalan, Augustin M.; Duhayon, Carine; Sutter, Jean-Pascal; Andruh, Marius; Chibotaru, Liviu F.; Inorganic chemistry 55 (2016) 12158–12171; doi:10.1021/acs.inorgchem.6b01669

data_4348810
_publ_section_title
;
 Synthesis, Crystal Structures, Magnetic Properties, and Theoretical
 Investigation of a New Series of
 Ni<sup>II</sup>-Ln<sup>III</sup>-W<sup>V</sup> Heterotrimetallics:
 Understanding the SMM Behavior of Mixed Polynuclear Complexes.
;
_journal_issue                   23
_journal_name_full               'Inorganic chemistry'
_journal_page_first              12158
_journal_page_last               12171
_journal_paper_doi               10.1021/acs.inorgchem.6b01669
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C27 H32 Lu N10 Ni O10 W'
_chemical_formula_weight         1074.15
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.9298(4)
_cell_length_b                   13.9422(7)
_cell_length_c                   30.8112(19)
_cell_measurement_reflns_used    26423
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.80
_cell_measurement_theta_min      2.29
_cell_volume                     3836.0(4)
_computing_cell_refinement       X-Area
_computing_data_collection       X-Area
_computing_data_reduction        X-Area
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.886
_diffrn_measured_fraction_theta_max 0.914
_diffrn_measurement_device_type  'STOE-IPDS II'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0947
_diffrn_reflns_av_unetI/netI     0.0738
_diffrn_reflns_Laue_measured_fraction_full 0.886
_diffrn_reflns_Laue_measured_fraction_max 0.914
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            19721
_diffrn_reflns_point_group_measured_fraction_full 0.906
_diffrn_reflns_point_group_measured_fraction_max 0.929
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.995
_diffrn_reflns_theta_min         2.375
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    6.092
_exptl_absorpt_correction_T_max  0.6352
_exptl_absorpt_correction_T_min  0.4766
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.860
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             2068
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         3.956
_refine_diff_density_min         -1.685
_refine_diff_density_rms         0.324
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.13(4)
_refine_ls_extinction_coef       0.0113(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     453
_refine_ls_number_reflns         7808
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0984
_refine_ls_R_factor_gt           0.0840
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1597P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2182
_refine_ls_wR_factor_ref         0.2316
_reflns_Friedel_coverage         0.818
_reflns_Friedel_fraction_full    0.931
_reflns_Friedel_fraction_max     0.949
_reflns_number_gt                6462
_reflns_number_total             7808
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01669_si_006.cif
_cod_data_source_block           shelx
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               4348810
_shelxl_version_number           2014-3
_shelx_res_checksum              40676
_shelx_hkl_checksum              88541