3,3'-[Ethane-1,2-diylbis(aminomethylene)]bis(pentane-2,4-dione) and the Nickel(II) Complex of a Condensation Product
König, Burkhard; Pelka, Mario; Dix, Ina; Jones, Peter G.; Acta Crystallographica Section C 54 (1998) 1468–1471; doi:10.1107/S0108270198009263

data_2007707
_publ_section_title
;
 3,3'-[Ethane-1,2-diylbis(aminomethylene)]bis(pentane-2,4-dione) and
 the Nickel(II) Complex of a Condensation Product
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1468
_journal_page_last               1471
_journal_paper_doi               10.1107/S0108270198009263
_journal_volume                  54
_journal_year                    1998
_chemical_formula_iupac          '[Ni (C16 H22 N4 O2)], 2C D Cl3'
_chemical_formula_moiety         '(C16 H22 N4 Ni O2) 2(C D Cl3)'
_chemical_formula_sum            'C18 H22 Cl6 D2 N4 Ni O2'
_chemical_formula_weight         601.83
_chemical_name_systematic
;
 [{6,13-diacetyl-5,12-dimethyl-1,4,8,11-tetraazacyclotetradeca-
 4,6,11,13-tetraenato(2-)}nickel(II)] deuterochloroform solvate (1:2)
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.542(3)
_cell_length_b                   9.406(3)
_cell_length_c                   30.213(8)
_cell_measurement_reflns_used    60
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      5.9
_cell_volume                     2427.5(13)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Fait, 1991)'
_computing_data_reduction        XSCANS
_computing_molecular_graphics    'XP (Siemens, 1994b)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       \w
_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  0.024
_diffrn_reflns_av_sigmaI/netI    0.0231
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            4120
_diffrn_reflns_theta_full        25.48
_diffrn_reflns_theta_max         25.48
_diffrn_reflns_theta_min         3.22
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 247
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.484
_exptl_absorpt_correction_T_max  0.690
_exptl_absorpt_correction_T_min  0.526
_exptl_absorpt_correction_type   '\y scans (XEMP; Siemens, 1994a)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.641
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.48
_refine_diff_density_min         -0.33
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   0.422(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    'H atoms: see below'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         3996
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.036
_refine_ls_R_factor_gt           0.031
_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^)+(0.0271P)^2^+2.643P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.069
_reflns_number_gt                3587
_reflns_number_total             3996
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bm1271.cif
_cod_data_source_block           2
_cod_original_cell_volume        2427.3(13)
_cod_original_formula_sum        'C18 H22 D2 Cl6 N4 Ni O2'
_cod_database_code               2007707