Tris(ethylenediamine-κ^2^<i>N</i>,<i>N</i>')nickel(II) bis(dimethyl phosphate)
Rafizadeh, Masoud; Saadati Moshtaghin, Hamid Reza; Amani, Vahid; Acta Crystallographica Section E 68 (2012) m1032–; doi:10.1107/S1600536812029984

data_2235861
_publ_section_title
;
 Tris(ethylenediamine-\k^2^<i>N</i>,<i>N</i>')nickel(II) bis(dimethyl
 phosphate)
;
_journal_coeditor_code           HY2566
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1032
_journal_paper_doi               10.1107/S1600536812029984
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Ni (C2 H8 N2)3] (C2 H6 O4 P)2'
_chemical_formula_moiety         'C6 H24 N6 Ni 2+, 2(C2 H6 O4 P -)'
_chemical_formula_sum            'C10 H36 N6 Ni O8 P2'
_chemical_formula_weight         489.08
_chemical_name_systematic
;
Tris(ethylenediamine-\k^2^<i>N</i>,<i>N</i>')nickel(II) bis(dimethyl phosphate)
;
_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                 90.156(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.2553(5)
_cell_length_b                   12.4913(5)
_cell_length_c                   18.1900(10)
_cell_measurement_reflns_used    9338
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.15
_cell_measurement_theta_min      2.74
_cell_volume                     2102.95(18)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2002)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'X-RED (Stoe & Cie, 2002)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 0.15
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Stoe IPDS-2T'
_diffrn_measurement_method       '\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  0.0308
_diffrn_reflns_av_sigmaI/netI    0.0309
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            9338
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         29.15
_diffrn_reflns_theta_min         2.74
_exptl_absorpt_coefficient_mu    1.123
_exptl_absorpt_correction_T_max  0.650
_exptl_absorpt_correction_T_min  0.590
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(X-SHAPE and X-RED; Stoe & Cie, 2002)'
_exptl_crystal_colour            Violet
_exptl_crystal_density_diffrn    1.545
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.38
_refine_diff_density_max         0.509
_refine_diff_density_min         -0.404
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         5205
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0336
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0434P)^2^+1.1522P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0821
_refine_ls_wR_factor_ref         0.0848
_reflns_number_gt                4555
_reflns_number_total             5205
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hy2566.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2235861
_cod_database_fobs_code          2235861