Further refinement of diaqua(1,7,11,17-tetraoxa-2,6,12,16-tetraazacycloeicosane-<i>N,N</i>',<i>N</i>'',<i>N</i>''')nickel(II) dichloride
Kuksa, Vladimir A.; Wardell, Solange M. S. V; Lin, Paul Kong Thoo; Howie, R. Alan; Acta Crystallographica Section E 58 (2002) m74–m76; doi:10.1107/S1600536802001915

data_2200858
_publ_section_title
;Further refinement of
 diaqua(1,7,11,17-tetraoxa-2,6,12,16-tetraazacycloeicosane-<i>N,N</i>',<i>N</i>'',<i>N</i>''')nickel(II)
 dichloride
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m74
_journal_page_last               m76
_journal_paper_doi               10.1107/S1600536802001915
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          '[Ni (C12 H28 N4 O4) (H2 O)2] Cl2'
_chemical_formula_moiety         'C12 H32 N4 Ni O6 2+, 2Cl 1-'
_chemical_formula_sum            'C12 H32 Cl2 N4 Ni O6'
_chemical_formula_weight         458.03
_chemical_name_systematic
;
2,6,12,16-Tetraaza-1,7,11,17-tetraoxacycloicosane-diaquanickel(II) dichloride
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.2480(18)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.4288(3)
_cell_length_b                   13.1426(5)
_cell_length_c                   10.2527(3)
_cell_measurement_reflns_used    15576
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.38
_cell_measurement_theta_min      2.03
_cell_volume                     978.23(6)
_computing_cell_refinement       MADNES
_computing_data_collection       'MADNES (Pflugrath & Messerschmidt, 1989)'
_computing_data_reduction        'ABSMAD (Karaulov, 1992)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full .997
_diffrn_measured_fraction_theta_max .997
_diffrn_measurement_device_type  'Delft Instruments FAST area-detector'
_diffrn_measurement_method       \f
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .0513
_diffrn_reflns_av_sigmaI/netI    .0250
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            15576
_diffrn_reflns_theta_full        26.38
_diffrn_reflns_theta_max         26.38
_diffrn_reflns_theta_min         2.03
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.300
_exptl_absorpt_correction_T_max  .823
_exptl_absorpt_correction_T_min  .710
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   '(DIFABS; Walker & Stuart, 1983)'
_exptl_crystal_colour            'light violet'
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             484
_exptl_crystal_size_max          .60
_exptl_crystal_size_mid          .15
_exptl_crystal_size_min          .15
_refine_diff_density_max         .310
_refine_diff_density_min         -.639
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         2090
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          .0282
_refine_ls_R_factor_gt           .0246
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0267P)^2^+0.4373P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          .0613
_refine_ls_wR_factor_ref         .0631
_reflns_number_gt                1892
_reflns_number_total             2090
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cf6147.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_hydrogens' value 'geom and difmap' was changed
to 'mixed'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        978.22(6)
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               2200858
_cod_database_fobs_code          2200858