Preparation and characterization of mononuclear Co, Ni, and Zn complexes of dinucleating macrocyclic hexaaza-dithiophenolate ligands and their open-chain derivatives.
Fritz, Thorsten; Steinfeld, Gunther; Käss, Steffen; Kersting, Berthold; Dalton transactions (Cambridge, England : 2003)  (2006) 3812–3821; doi:10.1039/b603740b

data_7007327
_publ_section_title
;
 Preparation and characterization of mononuclear Co, Ni, and Zn
 complexes of dinucleating macrocyclic hexaaza-dithiophenolate ligands
 and their open-chain derivatives.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3812
_journal_page_last               3821
_journal_paper_doi               10.1039/b603740b
_journal_year                    2006
_chemical_compound_source
;
Crystals were grown from acetonitrile.
;
_chemical_formula_structural
;
[Ni(L5)]
;
_chemical_formula_sum            'C21 H29 N3 Ni S2'
_chemical_formula_weight         446.30
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 96.70(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.320(4)
_cell_length_b                   7.583(2)
_cell_length_c                   15.183(3)
_cell_measurement_reflns_used    138
_cell_measurement_temperature    210(2)
_cell_measurement_theta_max      24
_cell_measurement_theta_min      10
_cell_volume                     2094.8(8)
_computing_cell_refinement       SMART
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    'ORTEP3 (FARRUGIA)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      210(2)
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  'BRUKER AXS'
_diffrn_measurement_method       hemisphere
_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  0.0778
_diffrn_reflns_av_sigmaI/netI    0.1223
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12760
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.12
_exptl_absorpt_coefficient_mu    1.137
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.77
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS, Sheldrick, 1996)'
_exptl_crystal_colour            block
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       red
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.644
_refine_diff_density_min         -0.783
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.972
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         4931
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.1336
_refine_ls_R_factor_gt           0.0524
_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^)+(0.0392P)^2^+1.2582P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0956
_refine_ls_wR_factor_ref         0.1270
_reflns_number_gt                2489
_reflns_number_total             4931
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b603740b.txt
_cod_data_source_block           5
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7007327