Azide Binding Controlled by Steric Interactions in Second Sphere. Synthesis, Crystal Structure, and Magnetic Properties of [Ni(II)2(L)(μ(1,1)-N3)][ClO4] (L = Macrocyclic N6S2 Ligand).
Jeremies, Alexander; Gruschinski, Sina; Meyer, Michel; Matulis, Vitaly; Ivashkevich, Oleg A.; Kobalz, Karolin; Kersting, Berthold; Inorganic chemistry 55 (2016) 1843–1853; doi:10.1021/acs.inorgchem.5b02743

data_4347117
_publ_section_title
;
 Azide Binding Controlled by Steric Interactions in Second Sphere.
 Synthesis, Crystal Structure, and Magnetic Properties of
 [Ni(II)2(L)(\m(1,1)-N3)][ClO4] (L = Macrocyclic N6S2 Ligand).
;
_journal_issue                   4
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1843
_journal_page_last               1853
_journal_paper_doi               10.1021/acs.inorgchem.5b02743
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C38 H64 Cl N9 Ni2 O4 S2'
_chemical_formula_weight         927.97
_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_space_group_name_H-M   'P 1 21/c 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                 105.73(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.929(3)
_cell_length_b                   23.299(5)
_cell_length_c                   13.836(3)
_cell_measurement_reflns_used    13670
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      24.3
_cell_measurement_theta_min      2.0
_cell_volume                     5253(2)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-AREA, STOE X-RED'
_computing_molecular_graphics    'ORTEP 3 (Farrugia, 1999)'
_computing_publication_material  'ORTEP 3 (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  STOE-IPDS-2T
_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  0.0388
_diffrn_reflns_av_sigmaI/netI    0.0495
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            33740
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.15
_exptl_absorpt_coefficient_mu    0.888
_exptl_absorpt_correction_T_max  0.9164
_exptl_absorpt_correction_T_min  0.9164
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            block
_exptl_crystal_density_diffrn    1.173
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       pale-green
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
;
_refine_diff_density_max         0.738
_refine_diff_density_min         -0.660
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.893
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         9228
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      0.934
_refine_ls_R_factor_all          0.0637
_refine_ls_R_factor_gt           0.0449
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0790P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1141
_refine_ls_wR_factor_ref         0.1190
_reflns_number_gt                6392
_reflns_number_total             9228
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b02743_si_002.cif
_cod_data_source_block           azsq
_cod_original_cell_volume        5253.3(18)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4347117