Geometrical isomerism in octahedral complexes arising from the presence of a fused ring on a triaza macrocycle
Comba, Peter; DeIuliis, Geoffry N.; Lawrance, Geoffrey A.; Luther, Stephan M.; Maeder, Marcel; Nolan, Annette L.; Robertson, Mark J.; Turner, Peter; Dalton Transactions  (2003) 2188–; doi:10.1039/b303515h

data_7013002
_publ_section_title
;
 Geometrical isomerism in octahedral complexes arising from the
 presence of a fused ring on a triaza macrocycle
;
_journal_issue                   11
_journal_name_full               'Dalton Transactions'
_journal_page_first              2188
_journal_paper_doi               10.1039/b303515h
_journal_year                    2003
_chemical_formula_sum            'C20 H42 N8 Ni O6'
_chemical_formula_weight         549.33
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 103.509(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.590(2)
_cell_length_b                   11.754(3)
_cell_length_c                   12.725(3)
_cell_measurement_reflns_used    986
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      25.774
_cell_measurement_theta_min      2.439
_cell_volume                     1249.3(5)
_computing_cell_refinement       'SAINT (Bruker,1995)'
_computing_data_collection       'SMART (Bruker,1995)'
_computing_data_reduction        'SAINT and XPREP (Bruker 1995)'
_computing_molecular_graphics
;
teXsan for Windows (MSC, 1997) 
xtal 3.6 (Hall,du Boulay, D.J. & Olthof-Hazekamp, R. 1999)
ORTEPII  (Johnson,C.K., 1976). 
WinGX (Farrugia, 1999)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare, et. al. 1997)'
_diffrn_ambient_temperature      294(2)
_diffrn_crystal_treatment
;
attached to a thin glass fibre
;
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0261
_diffrn_reflns_av_sigmaI/netI    0.0342
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11997
_diffrn_reflns_theta_full        26.41
_diffrn_reflns_theta_max         26.41
_diffrn_reflns_theta_min         2.39
_diffrn_standards_decay_%        0.0
_diffrn_standards_number         137
_exptl_absorpt_coefficient_mu    0.829
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.886
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            'pale pink'
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             588
_exptl_crystal_size_max          0.181
_exptl_crystal_size_mid          0.112
_exptl_crystal_size_min          0.074
_refine_diff_density_max         0.329
_refine_diff_density_min         -0.208
_refine_diff_density_rms         0.037
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.001(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         5026
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0294
_refine_ls_R_factor_gt           0.0258
_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^)+(0.0338P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0616
_refine_ls_wR_factor_ref         0.0634
_reflns_number_gt                4676
_reflns_number_total             5026
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b303515h.txt
_cod_data_source_block           gal1
_cod_original_cell_volume        1249.3(6)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7013002