Synthesis and Characterization of Two Polymorphic Crystalline Phases and an Amorphous Powder of Nickel(II) Bisimidazolate
Norberto Masciocchi; Fulvio Castelli; Paul M. Forster; Maya M. Tafoya; Anthony K. Cheetham; Inorganic Chemistry 42 (2003) 6147–6152; doi:10.1021/ic034619o

data_4314284
_publ_section_title
;
 Synthesis and Characterization of Two Polymorphic Crystalline Phases and
 an Amorphous Powder of Nickel(II) Bisimidazolate
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6147
_journal_page_last               6152
_journal_paper_doi               10.1021/ic034619o
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C6 H6 N4 Ni'
_chemical_formula_weight         192.87
_chemical_name_systematic        bisimidazolato-nickel(ii)
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.388(3)
_cell_length_b                   8.755(4)
_cell_length_c                   10.489(4)
_cell_measurement_temperature    293(2)
_cell_volume                     678.4(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Siemens Smart CCD'
_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  0.0615
_diffrn_reflns_av_sigmaI/netI    0.0347
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3753
_diffrn_reflns_theta_full        28.26
_diffrn_reflns_theta_max         28.26
_diffrn_reflns_theta_min         3.61
_exptl_absorpt_coefficient_mu    2.760
_exptl_crystal_colour            orange-yellow
_exptl_crystal_density_diffrn    1.888
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'elongated cubes'
_exptl_crystal_F_000             336
_exptl_crystal_size_max          80
_exptl_crystal_size_mid          60
_exptl_crystal_size_min          60
_refine_diff_density_max         0.394
_refine_diff_density_min         -0.252
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     60
_refine_ls_number_reflns         819
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0249
_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^+0.1722P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0519
_refine_ls_wR_factor_ref         0.0565
_reflns_number_gt                648
_reflns_number_total             819
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034619osi20030604_030654.cif
_cod_data_source_block           niimm
_cod_database_code               4314284