Bis[1-methoxy-2,2,2-tris(pyrazol-1-yl-κ<i>N</i>^2^)ethane]nickel(II) bis(trifluoromethanesulfonate) dihydrate
Lyubartseva, Ganna; Parkin, Sean; Mallik, Uma Prasad; Acta Crystallographica Section E 69 (2013) m532–m533; doi:10.1107/S1600536813024252

data_2238678
_publ_section_title
;
 Bis[1-methoxy-2,2,2-tris(pyrazol-1-yl-\k<i>N</i>^2^)ethane]nickel(II)
 bis(trifluoromethanesulfonate) dihydrate
;
_journal_coeditor_code           TK5252
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m532
_journal_page_last               m533
_journal_paper_doi               10.1107/S1600536813024252
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '[Ni (C12 H14 N6 O)2] (C F3 O3 S)2, 2H2 O'
_chemical_formula_moiety         'C24 H28 N12 Ni O2 2+, 2(C F3 O3 S -), 2(H2 O)'
_chemical_formula_sum            'C26 H32 F6 N12 Ni O10 S2'
_chemical_formula_weight         909.46
_chemical_name_systematic
;
Bis[1-methoxy-2,2,2-tris(pyrazol-1-yl-\k<i>N</i>^2^)ethane]nickel(II)
bis(trifluoromethanesulfonate) dihydrate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                110.3990(10)
_cell_angle_beta                 103.6650(10)
_cell_angle_gamma                97.3170(10)
_cell_formula_units_Z            1
_cell_length_a                   8.5582(2)
_cell_length_b                   9.6515(2)
_cell_length_c                   12.2347(2)
_cell_measurement_reflns_used    25674
_cell_measurement_temperature    90.0(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     895.66(3)
_computing_cell_refinement       'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008<i>b</i>)'
_computing_publication_material  'SHELXL2013 (Sheldrick, 2008<i>b</i>)'
_computing_structure_refinement  'SHELXL2013 (Sheldrick, 2008<i>b</i>)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008<i>b</i>)'
_diffrn_ambient_temperature      90.0(2)
_diffrn_detector_area_resol_mean 9.1
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_diffrn_measurement_method       '\f and \w scans at fixed \c = 55\%'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            25573
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         1.863
_exptl_absorpt_coefficient_mu    0.762
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.760
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2008<i>a</i>)'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.686
_exptl_crystal_description       block
_exptl_crystal_F_000             466
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.469
_refine_diff_density_min         -0.494
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         4095
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0291
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0311P)^2^+0.6676P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0701
_refine_ls_wR_factor_ref         0.0719
_reflns_number_gt                3708
_reflns_number_total             4095
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            tk5252.cif
_cod_data_source_block           I
_cod_database_code               2238678
_shelx_estimated_absorpt_t_min   0.827
_shelx_estimated_absorpt_t_max   0.894
_shelx_hkl_checksum              29507
_shelx_res_checksum              32268
_shelxl_version_number           .2013