(<i>meso</i>-5,5,7,12,12,14-Hexamethyl-1,4,8,11-tetraazacyclotetradecane)nickel(II) bis[<i>O</i>,<i>O</i>'-bis(4-methylphenyl) thiophosphate]
Xiang, Yang-Guang; Xie, Bin; Zou, Li-Ke; Feng, Jian-Shen; Lai, Chuan; Acta Crystallographica Section E 67 (2011) m59–; doi:10.1107/S1600536810051184

data_2228820
_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>'-bis(4-methylphenyl) thiophosphate]
;
_journal_coeditor_code           NC2207
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m59
_journal_paper_doi               10.1107/S1600536810051184
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Ni (C16 H36 N4)] (C14 H14 O3 P S)2'
_chemical_formula_moiety         'C16 H36 N4 Ni 2+, 2(C14 H14 O3 P S -)'
_chemical_formula_sum            'C44 H64 N4 Ni O6 P2 S2'
_chemical_formula_weight         929.76
_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>'-bis(4-methylphenyl) thiophosphate]
;
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.85(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.977(2)
_cell_length_b                   16.360(3)
_cell_length_c                   12.767(3)
_cell_measurement_reflns_used    7232
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.90
_cell_measurement_theta_min      2.20
_cell_volume                     2284.5(8)
_computing_cell_refinement       'CrystalClear (Rigaku, 2005)'
_computing_data_collection       'CrystalClear (Rigaku, 2005)'
_computing_data_reduction        'CrystalClear (Rigaku, 2005)'
_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      113(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Rigaku Saturn CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1013
_diffrn_reflns_av_sigmaI/netI    0.1356
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18654
_diffrn_reflns_theta_full        27.91
_diffrn_reflns_theta_max         27.91
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    0.637
_exptl_absorpt_correction_T_max  0.8726
_exptl_absorpt_correction_T_min  0.8622
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrystalClear; Rigaku, 2005)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             988
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.974
_refine_diff_density_min         -0.914
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         5376
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.0852
_refine_ls_R_factor_gt           0.0529
_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^)+(0.0244P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1121
_refine_ls_wR_factor_ref         0.1217
_reflns_number_gt                2665
_reflns_number_total             5376
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            nc2207.cif
_cod_data_source_block           I
_cod_original_cell_volume        2284.6(8)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2228820
_cod_database_fobs_code          2228820