Huge Magnetic Anisotropy in a Trigonal-Pyramidal Nickel(II) Complex.
Gómez-Coca, Silvia; Cremades, Eduard; Aliaga-Alcalde, Núria; Ruiz, Eliseo; Inorganic chemistry 53 (2014) 676–678; doi:10.1021/ic402256v

data_4337082
_publ_section_title
;
 Huge Magnetic Anisotropy in a Trigonal-Pyramidal Nickel(II) Complex.
;
_journal_issue                   2
_journal_name_full               'Inorganic chemistry'
_journal_page_first              676
_journal_page_last               678
_journal_paper_doi               10.1021/ic402256v
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C39 H73 K2 N9 Ni2 O7'
_chemical_formula_sum            'C39 H73 K2 N9 Ni2 O7'
_chemical_formula_weight         975.68
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.26(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   18.750(11)
_cell_length_b                   9.636(5)
_cell_length_c                   14.324(4)
_cell_measurement_reflns_used    290
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      31
_cell_measurement_theta_min      3
_cell_volume                     2584(2)
_computing_cell_refinement       'AUTOMAR (Claudio Klein, 2007)'
_computing_data_collection       'MARXDS (Claudio Klein, 2005)'
_computing_data_reduction        'MARSCALE (Claudio Klein, 2007)'
_computing_molecular_graphics    'ORTEP (Brueggermann and Smith, 1990)'
_computing_publication_material  'PLATON (Spek, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.793
_diffrn_measurement_device_type  'MAR345 with image plate detector'
_diffrn_measurement_method       'phi scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_sigmaI/netI    0.0366
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11649
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         31.92
_diffrn_reflns_theta_min         1.42
_exptl_absorpt_coefficient_mu    0.940
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.92
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_density_diffrn    1.254
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.843
_refine_diff_density_min         -0.610
_refine_diff_density_rms         0.207
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_coef       0.0154(14)
_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   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         6574
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.766
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0389
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0663P)^2^+0.5455P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1088
_refine_ls_wR_factor_ref         0.1172
_reflns_number_gt                5958
_reflns_number_total             6574
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic402256v_si_002.cif
_cod_data_source_block           nuom142a
_cod_original_sg_symbol_H-M      C2
_cod_database_code               4337082