Synthesis, Crystal-Structure Determination and Magnetic Properties of Two New Transition-Metal Carbodiimides: CoNCN and NiNCN
Manuel Krott; Xiaohui Liu; Boniface P. T. Fokwa; Manfred Speldrich; Heiko Lueken; Richard Dronskowski; Inorganic Chemistry 46 (2007) 2204–2207; doi:10.1021/ic062051o

data_4307549
_publ_contact_author_address
;    
Institute of Inorganic Chemistry
RWTH Aachen University     
D-52056 Aachen
Germany
;
_publ_contact_author_email       drons@HAL9000.ac.rwth-aachen.de
_publ_contact_author_fax         00492418092642
_publ_contact_author_name        'Prof. Richard Dronskowski '
_publ_contact_author_phone       00492418093642
_publ_section_title
;
Synthesis, Crystal-Structure Determination and Magnetic Properties of Two
New Transition-Metal Carbodiimides: CoNCN and NiNCN
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2204
_journal_page_last               2207
_journal_paper_doi               10.1021/ic062051o
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C N2 Ni'
_chemical_formula_weight         98.74
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           194
_symmetry_cell_setting           hexagonal
_symmetry_Int_Tables_number      194
_symmetry_space_group_name_Hall  '-P 6c 2c'
_symmetry_space_group_name_H-M   'P 63/m m c'
_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                120.00
_cell_formula_units_Z            2
_cell_length_a                   3.1533(8)
_cell_length_b                   3.1533(8)
_cell_length_c                   9.272(3)
_cell_measurement_temperature    293(2)
_cell_volume                     79.84(4)
_computing_cell_refinement       'SMART (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    'Diamond 2.1c (K. Brandenburg, 1999)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.907
_diffrn_measured_fraction_theta_max 0.907
_diffrn_measurement_device_type  'Brucker APEX CCD area detector'
_diffrn_measurement_method       'integretion method'
_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  0.2101
_diffrn_reflns_av_sigmaI/netI    0.0798
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            1493
_diffrn_reflns_theta_full        35.99
_diffrn_reflns_theta_max         35.99
_diffrn_reflns_theta_min         7.48
_exptl_absorpt_coefficient_mu    11.574
_exptl_absorpt_correction_T_max  0.892
_exptl_absorpt_correction_T_min  0.654
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS(Bruker, 2001)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    4.107
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             96
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.735
_refine_diff_density_min         -1.686
_refine_diff_density_rms         0.406
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.441
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     6
_refine_ls_number_reflns         94
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.441
_refine_ls_R_factor_all          0.1397
_refine_ls_R_factor_gt           0.1045
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+3.1852P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1543
_refine_ls_wR_factor_ref         0.1638
_reflns_number_gt                75
_reflns_number_total             94
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic062051osi20061026_062238.cif
_cod_data_source_block           NiNCN
_cod_original_cell_volume        79.85(4)
_cod_database_code               4307549