(<i>meso</i>-5,7,7,12,14,14-Hexamethyl-1,4,8,11-tetraazacyclotetradeca-4,11-diene)nickel(II) bis[<i>O</i>,<i>O</i>'-bis(4-methylphenyl) dithiophosphate]
Xie, Bin; Xiang, Yang-Guang; Zou, Li-Ke; Chang, Xiu-Li; Ji, Chang-You; Acta Crystallographica Section E 65 (2009) m1053–; doi:10.1107/S1600536809030955

data_2223046
_publ_section_title
;(<i>meso</i>-5,7,7,12,14,14-Hexamethyl-1,4,8,11-tetraazacyclotetradeca-4,11-diene)nickel(II)
 bis[<i>O</i>,<i>O</i>'-bis(4-methylphenyl) dithiophosphate]
;
_journal_coeditor_code           DN2479
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1053
_journal_paper_doi               10.1107/S1600536809030955
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Ni (C16 H32 N4)] (C14 H14 O2 P S2)2'
_chemical_formula_moiety         'C16 H32 N4 Ni 2+, 2(C14 H14 O2 P S2 -) '
_chemical_formula_sum            'C44 H60 N4 Ni O4 P2 S4'
_chemical_formula_weight         957.85
_chemical_name_systematic
;
(<i>meso</i>-5,7,7,12,14,14-Hexamethyl-1,4,8,11-tetraazacyclotetradeca-4,11-
diene)nickel(II) bis[<i>O</i>,<i>O</i>'-bis(4-methylphenyl) dithiophosphate]
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                80.4180(10)
_cell_angle_beta                 81.3330(10)
_cell_angle_gamma                69.8360(10)
_cell_formula_units_Z            1
_cell_length_a                   8.0044(6)
_cell_length_b                   10.0996(8)
_cell_length_c                   16.4004(12)
_cell_measurement_reflns_used    3628
_cell_measurement_temperature    278(2)
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      2.37
_cell_volume                     1220.95(16)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'Ortep-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      278(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0124
_diffrn_reflns_av_sigmaI/netI    0.0224
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6525
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    0.677
_exptl_absorpt_correction_T_max  0.9354
_exptl_absorpt_correction_T_min  0.8878
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             506
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.499
_refine_diff_density_min         -0.335
_refine_ls_extinction_coef       0.0094(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         4305
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0319
_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^)+(0.0404P)^2^+0.4007P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0810
_refine_ls_wR_factor_ref         0.0852
_reflns_number_gt                3756
_reflns_number_total             4305
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            dn2479.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               2223046
_cod_database_fobs_code          2223046