(<i>meso</i>-5,5,7,12,12,14-Hexamethyl-1,4,8,11-tetraazacyclotetradecane)nickel(II) bis(<i>O</i>,<i>O</i>'-dibenzyl dithiophosphate)
Xie, Bin; Zou, Li-Ke; He, Yi-Guo; Feng, Jian-Shen; Zhang, Xiu-Lan; Acta Crystallographica Section E 64 (2008) m622–; doi:10.1107/S1600536808008398

data_2218095
_publ_section_title
;(<i>meso</i>-5,5,7,12,12,14-Hexamethyl-1,4,8,11-tetraazacyclotetradecane)nickel(II)
 bis(<i>O</i>,<i>O</i>'-dibenzyl dithiophosphate)
;
_journal_coeditor_code           DN2324
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m622
_journal_paper_doi               10.1107/S1600536808008398
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Ni (C16 H36 N4)] (C14 H14 O2 P S2)2'
_chemical_formula_moiety         'C16 H36 N4 Ni 2+, 2(C14 H14 O2 P S2 -)'
_chemical_formula_sum            'C44 H64 N4 Ni O4 P2 S4'
_chemical_formula_weight         961.88
_chemical_name_systematic
;
(<i>meso</i>-5,5,7,12,12,14-Hexamethyl-1,4,8,11-
tetraazacyclotetradecane)nickel(II)
bis(<i>O</i>,<i>O</i>'-dibenzyl dithiophosphate)
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.11(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.371(5)
_cell_length_b                   14.917(5)
_cell_length_c                   9.964(4)
_cell_measurement_reflns_used    19
_cell_measurement_temperature    290(2)
_cell_measurement_theta_max      5.51
_cell_measurement_theta_min      4.39
_cell_volume                     2369.9(15)
_computing_cell_refinement       'CAD-4 Software (Enraf--Nonius, 1989)'
_computing_data_collection       'CAD-4 Software (Enraf--Nonius, 1989)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      290(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Enraf--Nonius CAD-4'
_diffrn_measurement_method       \w/2\q
_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  0.0210
_diffrn_reflns_av_sigmaI/netI    0.0544
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5571
_diffrn_reflns_theta_full        25.52
_diffrn_reflns_theta_max         25.52
_diffrn_reflns_theta_min         1.28
_diffrn_standards_decay_%        1.085
_diffrn_standards_interval_count 300
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.698
_exptl_absorpt_correction_T_max  0.7872
_exptl_absorpt_correction_T_min  0.7676
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North <i>et al.</i>,  1968)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1020
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.36
_refine_diff_density_max         0.521
_refine_diff_density_min         -0.336
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         4393
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0915
_refine_ls_R_factor_gt           0.0491
_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^)+(0.0689P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1146
_refine_ls_wR_factor_ref         0.1271
_reflns_number_gt                2880
_reflns_number_total             4393
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            dn2324.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2218095
_cod_database_fobs_code          2218095