Characterization of two conformers in the co-ordination chemistry of 3,4-bis(cyanamido)cyclobutane-1,2-dione dianion: syntheses, crystal structures, and electrochemical study of nickel(ii) complexes
Galibert, Anne Marie; Cortadellas, Olivier; Soula, Brigitte; Donnadieu, Bruno; Fabre, Paul-Louis; Journal of the Chemical Society, Dalton Transactions  (2002) 3743–; doi:10.1039/b202085h

data_7011596
_publ_section_title
;
 Characterization of two conformers in the co-ordination chemistry of
 3,4-bis(cyanamido)cyclobutane-1,2-dione dianion: syntheses, crystal
 structures, and electrochemical study of nickel(ii) complexes
;
_journal_issue                   19
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3743
_journal_paper_doi               10.1039/b202085h
_journal_year                    2002
_chemical_formula_sum            'C9 H18 N6 Ni O9'
_chemical_formula_weight         413.00
_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                99.044(5)
_cell_angle_beta                 90.794(5)
_cell_angle_gamma                105.502(5)
_cell_formula_units_Z            2
_cell_length_a                   6.966(5)
_cell_length_b                   10.812(5)
_cell_length_c                   11.699(5)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      23.2
_cell_measurement_theta_min      2.35
_cell_volume                     837.1(8)
_computing_cell_refinement       'Stoe IPDS software (Stoe, 1996)'
_computing_data_collection       'Stoe IPDS software (Stoe, 1996)'
_computing_data_reduction        'XRED (Stoe, 1.08, 1996)'
_computing_molecular_graphics    'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1992)'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device       'Stoe IPDS'
_diffrn_measurement_method       \f
_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  0.0539
_diffrn_reflns_av_sigmaI/netI    0.0611
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6228
_diffrn_reflns_theta_full        23.25
_diffrn_reflns_theta_max         23.25
_diffrn_reflns_theta_min         2.42
_diffrn_standards_decay_%        <0.1
_diffrn_standards_interval_time  'every frame'
_diffrn_standards_number         200
_exptl_absorpt_coefficient_mu    1.217
_exptl_absorpt_correction_T_max  0.780
_exptl_absorpt_correction_T_min  0.370
_exptl_absorpt_correction_type   semi-empirical
_exptl_crystal_colour            'yellow green'
_exptl_crystal_density_diffrn    1.639
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             428
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.912
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.966
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         2273
_refine_ls_number_restraints     91
_refine_ls_restrained_S_all      0.948
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0380
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0535P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0836
_refine_ls_wR_factor_ref         0.0929
_reflns_number_gt                1631
_reflns_number_total             2273
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b202085h.txt
_cod_data_source_block           (2)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7011596
_computing_corr_abs              DIFABS