Preparation of an enantiomerically pure helical nickel(II) complex using a new chiral tetradentate ligand derived from an industrial waste material †
Pennemann, Helmut; Wassmann, Suzanne; Wilken, Jörg; Gröger, Harald; Wallbaum, Sabine; Kossenjans, Michael; Haase, Detlev; Saak, Wolfgang; Pohl, Siegfried; Martens, Jürgen; Journal of the Chemical Society, Dalton Transactions  (2000) 2467–; doi:10.1039/b002130j

data_7009576
_publ_section_title
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 Preparation of an enantiomerically pure helical nickel(II) complex
 using a new chiral tetradentate ligand derived from an industrial
 waste material&#x200A;&#x2020;
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_journal_issue                   14
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2467
_journal_paper_doi               10.1039/b002130j
_journal_year                    2000
_chemical_formula_sum            'C18 H30 N2 Ni O6'
_chemical_formula_weight         429.13
_chemical_name_common            '[Ni(edda)(H2O)]xH2O'
_chemical_temperature_decomposition_gt 447.15
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 104.860(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.3020(10)
_cell_length_b                   15.2160(10)
_cell_length_c                   8.9250(10)
_cell_measurement_reflns_used    33
_cell_measurement_temperature    295(2)
_cell_volume                     958.47(19)
_computing_cell_refinement       'STADI 4 (Stoe, 1993)'
_computing_data_collection       'STADI4 (Stoe, 1993)'
_computing_data_reduction        'XRED (Stoe, 1993)'
_computing_molecular_graphics    'Schakal97 (E. Keller, 1997)'
_computing_publication_material  'SHELX-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTL Plus'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Stoe AED2'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0272
_diffrn_reflns_av_sigmaI/netI    0.0206
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            2336
_diffrn_reflns_theta_full        27.01
_diffrn_reflns_theta_max         27.01
_diffrn_reflns_theta_min         3.23
_diffrn_standards_interval_time  45
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.049
_exptl_absorpt_correction_T_max  0.2902
_exptl_absorpt_correction_T_min  0.2015
_exptl_absorpt_correction_type   'empirical psi-scan'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_description       'square crystals'
_exptl_crystal_F_000             448
_exptl_crystal_size_max          .6
_exptl_crystal_size_mid          .6
_exptl_crystal_size_min          .4
_refine_diff_density_max         0.651
_refine_diff_density_min         -0.365
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.016(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         2172
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0349
_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^)+(0.0700P)^2^+0.1936P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0910
_refine_ls_wR_factor_ref         0.0919
_reflns_number_gt                2104
_reflns_number_total             2172
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b002130j.txt
_cod_data_source_block           '[Ni(edda)(H2O)]xH2O'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' tag was changed to
'_chemical_temperature_decomposition_gt' since the value was
specified 'more than' ('>') a certain temperature. The value '>174 C
(decomposition)' was changed to '447.15' - it was converted from
degrees Celsius(C) to Kelvins(K).

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        958.47(18)
_cod_original_sg_symbol_H-M      P21
_cod_database_code               7009576