(<i>C-meso-N-meso</i>-5,12-Dimethyl-7,14-diphenyl-1,4,8,11-tetraazacyclotetradeca-4,11-diene)nickel(II) bis[<i>O</i>,<i>O</i>'-bis(4-methylphenyl) dithiophosphate]
Zou, Li-Ke; Xie, Bin; Feng, Jian-Shen; Lai, Chuan; Acta Crystallographica Section E 66 (2010) m1663–m1664; doi:10.1107/S160053681004849X

data_2228460
_publ_section_title
;
 (<i>C-meso-N-meso</i>-5,12-Dimethyl-7,14-diphenyl-1,4,8,11-tetraazacyclotetradeca-4,11-diene)nickel(II)
 bis[<i>O</i>,<i>O</i>'-bis(4-methylphenyl) dithiophosphate]
;
_journal_coeditor_code           LH5160
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1663
_journal_page_last               m1664
_journal_paper_doi               10.1107/S160053681004849X
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Ni (C24 H32 N4)] (C14 H14 O2 P S2)2'
_chemical_formula_moiety         'C24 H32 N4 Ni 2+, 2(C14 H14 O2 P S2 -)'
_chemical_formula_sum            'C52 H60 N4 Ni O4 P2 S4'
_chemical_formula_weight         1053.93
_chemical_name_systematic
;
(<i>C-meso-N-meso</i>-5,12-Dimethyl-7,14-diphenyl-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           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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 106.900(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.04828(18)
_cell_length_b                   19.6896(4)
_cell_length_c                   13.5112(3)
_cell_measurement_reflns_used    5452
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      29.1979
_cell_measurement_theta_min      2.9555
_cell_volume                     2557.70(9)
_computing_cell_refinement       'CrysAlis PRO CCD (Oxford Diffraction, 2009)'
_computing_data_collection       'CrysAlis PRO CCD (Oxford Diffraction, 2009)'
_computing_data_reduction        'CrysAlis PRO RED (Oxford Diffraction, 2009)'
_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      150.0
_diffrn_detector_area_resol_mean 16.0874
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur Eos'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_av_sigmaI/netI    0.0420
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11501
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.96
_exptl_absorpt_coefficient_mu    0.654
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.93021
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlis PRO RED; Oxford Diffraction, 2009)'
_exptl_crystal_colour            pale-violet
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1108
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.387
_refine_diff_density_min         -0.278
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         5232
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0357
_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^)+(0.0330P)^2^+1.1390P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0781
_refine_ls_wR_factor_ref         0.0848
_reflns_number_gt                4326
_reflns_number_total             5232
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh5160.cif
_cod_data_source_block           I
_cod_original_cell_volume        2557.69(9)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2228460
_cod_database_fobs_code          2228460