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_7007329
_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 methanol.
;
_chemical_formula_structural
;
[NiH2(L2)](ClO4)2MeOH
;
_chemical_formula_sum            'C39 H70 Cl2 N6 Ni O9 S2'
_chemical_formula_weight         960.74
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 93.04(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.073(3)
_cell_length_b                   17.070(3)
_cell_length_c                   19.323(4)
_cell_measurement_reflns_used    87
_cell_measurement_temperature    210(2)
_cell_measurement_theta_max      23
_cell_measurement_theta_min      8
_cell_volume                     4635.4(16)
_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  0.0391
_diffrn_reflns_av_sigmaI/netI    0.0797
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            28635
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    0.681
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.85
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS, Sheldrick, 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.922
_refine_diff_density_min         -0.610
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.890
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     560
_refine_ls_number_reflns         10921
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      0.910
_refine_ls_R_factor_all          0.0948
_refine_ls_R_factor_gt           0.0463
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0689P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1096
_refine_ls_wR_factor_ref         0.1319
_reflns_number_gt                6237
_reflns_number_total             10921
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b603740b.txt
_cod_data_source_block           7_ClO4
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7007329