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_7013003
_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 Cl3 Cr N6 O4.88'
_chemical_formula_weight         602.95
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      18
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_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            8
_cell_length_a                   18.936(4)
_cell_length_b                   29.495(5)
_cell_length_c                   11.545(2)
_cell_measurement_reflns_used    978
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      22.125
_cell_measurement_theta_min      2.866
_cell_volume                     6448(2)
_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 0.987
_diffrn_measured_fraction_theta_max 0.987
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.0605
_diffrn_reflns_av_sigmaI/netI    0.0505
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            78427
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.38
_diffrn_standards_decay_%        0.0
_diffrn_standards_number         250
_exptl_absorpt_coefficient_mu    0.638
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.937
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2544
_exptl_crystal_size_max          0.169
_exptl_crystal_size_mid          0.134
_exptl_crystal_size_min          0.134
_refine_diff_density_max         1.261
_refine_diff_density_min         -0.451
_refine_diff_density_rms         0.130
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.568
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     632
_refine_ls_number_reflns         15650
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.568
_refine_ls_R_factor_all          0.1134
_refine_ls_R_factor_gt           0.0664
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.05P)^2^+5.0P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1773
_refine_ls_wR_factor_ref         0.1943
_reflns_number_gt                10662
_reflns_number_total             15616
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b303515h.txt
_cod_data_source_block           gal3
_cod_original_sg_symbol_H-M      'P 21212'
_cod_database_code               7013003