(<i>meso</i>-5,5,7,12,12,14-Hexamethyl-1,4,8,11-tetraazacyclotetradecane)nickel(II) bis[<i>O</i>,<i>O</i>'-(1,2-phenylene) dithiophosphate]
Zou, Li-Ke; Lu, Yan; Cheng, Jie; He, Xi-Yang; Xie, Bin; Acta Crystallographica Section E 67 (2011) m1902–; doi:10.1107/S1600536811050951

data_2233027
_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>'-(1,2-phenylene) dithiophosphate]
;
_journal_coeditor_code           XU5399
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1902
_journal_paper_doi               10.1107/S1600536811050951
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Ni (C16 H36 N4)] (C6 H4 O2 P S2)2'
_chemical_formula_moiety         'C16 H36 N4 Ni 2+, 2(C6 H4 O2 P S2 -)'
_chemical_formula_sum            'C28 H44 N4 Ni O4 P2 S4'
_chemical_formula_weight         749.56
_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>'-(1,2-phenylene)
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                 101.029(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.0012(15)
_cell_length_b                   20.500(3)
_cell_length_c                   9.6682(17)
_cell_measurement_reflns_used    2892
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      24.47
_cell_measurement_theta_min      2.37
_cell_volume                     1751.1(5)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'SMART (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_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      103(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART 1000 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  0.0264
_diffrn_reflns_av_sigmaI/netI    0.0297
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            9094
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.99
_exptl_absorpt_coefficient_mu    0.922
_exptl_absorpt_correction_T_max  0.8516
_exptl_absorpt_correction_T_min  0.8090
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             788
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.395
_refine_diff_density_min         -0.267
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     197
_refine_ls_number_reflns         3103
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0355
_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^)+(0.0391P)^2^+0.6628P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0810
_refine_ls_wR_factor_ref         0.0874
_reflns_number_gt                2504
_reflns_number_total             3103
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            xu5399.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2233027
_cod_database_fobs_code          2233027