Tetranuclear nickel(II) complexes with genuine μ3-1,1,3 and μ4-1,1,3,3 azide bridges
Meyer, Franc; Kircher, Peter; Pritzkow, Hans; Chemical Communications (Cambridge, United Kingdom)  (2003) 774–775; doi:10.1039/b211486k

data_7104011
_publ_section_title
;
 Tetranuclear nickel(II) complexes with genuine \m3-1,1,3 and
 \m4-1,1,3,3 azide bridges
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   6
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              774
_journal_page_last               775
_journal_paper_doi               10.1039/b211486k
_journal_year                    2003
_chemical_formula_sum            'C46.25 H89.5 Cl2 N17 Ni4 O10.75 S8'
_chemical_formula_weight         1618.07
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 113.59(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.140(4)
_cell_length_b                   16.348(3)
_cell_length_c                   22.316(5)
_cell_measurement_temperature    200
_cell_volume                     7068(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'NONIUS KAPPA CCD'
_diffrn_measurement_method       'O-Scan    '
_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  0.0446
_diffrn_reflns_av_sigmaI/netI    0.0661
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            43065
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    1.424
_exptl_absorpt_correction_type   experimental
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3384
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.970
_refine_diff_density_min         -0.670
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     887
_refine_ls_number_reflns         18801
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0839
_refine_ls_R_factor_gt           0.0423
_refine_ls_shift/su_max          0.909
_refine_ls_shift/su_mean         0.022
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0570P)^2^+0.4765P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1033
_refine_ls_wR_factor_ref         0.1167
_reflns_number_gt                12291
_reflns_number_total             18801
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b211486k.txt
_cod_data_source_block           fmmo
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_original_formula_sum
'C44 H85 N17 O10 S8 Cl2 Ni4, 0.75(CH3 CO CH3)'
_cod_database_code               7104011