Hexaaquanickel(II) disulfato(1,4,8,11-tetraazacyclotetradecane)nickelate(II) dihydrate
Churchard, Andrew James; Cyrański, Michał Ksawery; Grochala, Wojciech; Acta Crystallographica Section C 66 (2010) m263–m265; doi:10.1107/S0108270110031598

data_2017857
_publ_section_title
;
 Hexaaquanickel(II)
 disulfato(1,4,8,11-tetraazacyclotetradecane)nickelate(II) dihydrate
;
_journal_coeditor_code           SF3137
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m263
_journal_page_last               m265
_journal_paper_doi               10.1107/S0108270110031598
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac
'[Ni (H2 O)6] [Ni (C10 H24 N4)  (S O4)2], 2 H2 O'
_chemical_formula_moiety
'C10 H24 N4 Ni1 O8 S2 2-, Ni H12 O6 2+, 2(H2 O)'
_chemical_formula_sum            'C10 H40 N4 Ni2 O16 S2'
_chemical_formula_weight         654.00
_chemical_name_systematic
;
hexaaqua nickel(II) bissulfato-1,4,8,11-tetraazacyclotetradecane nickelate(II)
dihydrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                98.558(7)
_cell_angle_beta                 99.869(8)
_cell_angle_gamma                91.640(7)
_cell_formula_units_Z            1
_cell_length_a                   8.0997(7)
_cell_length_b                   8.4360(6)
_cell_length_c                   9.3521(9)
_cell_measurement_reflns_used    11856
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.6974
_cell_measurement_theta_min      2.5517
_cell_volume                     621.59(9)
_computing_cell_refinement       'CrysAlis CCD? (Oxford Diffraction, 2004)'
_computing_data_collection       'CrysAlis CCD? (Oxford Diffraction, 2004)'
_computing_data_reduction        'CrysAlis RED? (Oxford Diffraction, 2004)'
_computing_publication_material  'Mercury (CCDC, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.6479
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'KM4 CCD'
_diffrn_measurement_method       '\w scan'
_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  0.0249
_diffrn_reflns_av_sigmaI/netI    0.0284
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            10420
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.56
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    1.760
_exptl_absorpt_correction_T_max  0.9171
_exptl_absorpt_correction_T_min  0.8436
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis RED; Oxford Diffraction, 2004)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.747
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             344
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.292
_refine_diff_density_min         -0.400
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.945
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     197
_refine_ls_number_reflns         2438
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.945
_refine_ls_R_factor_all          0.0247
_refine_ls_R_factor_gt           0.0179
_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^)+(0.0226P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0394
_refine_ls_wR_factor_ref         0.0402
_reflns_number_gt                2010
_reflns_number_total             2438
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sf3137.cif
_cod_data_source_block           I
_cod_original_sg_symbol_Hall     -P1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               2017857
_cod_database_fobs_code          2017857