Ethylenediammonium tetrakis({2,2'-[ethane-1,2-diylbis(nitrilomethylidyne)]diphenolato}nickel(II)) bis(perchlorate) dimethylformamide monosolvate
Assey, Gervas; Gultneh, Yilma; Butcher, Ray J.; Acta Crystallographica Section E 66 (2010) m654–m655; doi:10.1107/S1600536810017162

data_2226290
_publ_section_title
;
 Ethylenediammonium
 tetrakis({2,2'-[ethane-1,2-diylbis(nitrilomethylidyne)]diphenolato}nickel(II))
 bis(perchlorate) dimethylformamide monosolvate
;
_journal_coeditor_code           SJ2787
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m654
_journal_page_last               m655
_journal_paper_doi               10.1107/S1600536810017162
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac
'(C2 H10 N2) [Ni (C16 H14 N2 O2)]4, (Cl O4)2, C3 H7 N O'
_chemical_formula_moiety
'C2 H10 N2 2+, 4(C16 H14 N2 Ni O2), 2(Cl O4 -), C3 H7 N O'
_chemical_formula_sum            'C69 H73 Cl2 N11 Ni4 O17'
_chemical_formula_weight         1634.12
_chemical_name_systematic
;
Ethylenediammonium
tetrakis({2,2'-[ethane-1,2-diylbis(nitrilomethylidyne)]diphenolato}nickel(II))
bis(perchlorate) dimethylformamide monosolvate
;
_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                85.990(5)
_cell_angle_beta                 86.506(5)
_cell_angle_gamma                62.963(8)
_cell_formula_units_Z            2
_cell_length_a                   15.0209(11)
_cell_length_b                   15.0492(13)
_cell_length_c                   18.2709(8)
_cell_measurement_reflns_used    14342
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      34.7215
_cell_measurement_theta_min      4.5108
_cell_volume                     3667.8(5)
_computing_cell_refinement
;
CrysAlis RED (Oxford Diffraction, 2007)
;
_computing_data_collection
;
CrysAlis CCD (Oxford Diffraction, 2007)
;
_computing_data_reduction
;
CrysAlis RED (Oxford Diffraction, 2007)
;
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 10.5081
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Oxford Diffraction Gemini R'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_sigmaI/netI    0.0453
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            31940
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.21
_diffrn_reflns_theta_min         4.51
_diffrn_standards_decay_%        <2%
_diffrn_standards_interval_count 50
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.158
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83228
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis RED; Oxford Diffraction, 2007)
;
_exptl_crystal_colour            'translucent red-brown'
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'thick needle'
_exptl_crystal_F_000             1692
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.564
_refine_diff_density_min         -0.323
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.954
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     936
_refine_ls_number_reflns         13062
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      0.959
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0389
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0701P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1045
_refine_ls_wR_factor_ref         0.1096
_reflns_number_gt                9248
_reflns_number_total             13062
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sj2787.cif
_cod_data_source_block           I
_cod_original_cell_volume        3667.8(4)
_cod_database_code               2226290
_cod_database_fobs_code          2226290