Synthesis and X-ray structures of cadmium-containing dinuclear double helicates derived from ligands containing N-oxide units
Bokolinis, Georgios; Riis-Johannessen, T.; Jeffery, John C.; Rice, Craig R.; New Journal of Chemistry 32 (2008) 115–; doi:10.1039/b711039a

data_7051803
_publ_section_title
;
 Synthesis and X-ray structures of cadmium-containing dinuclear double
 helicates derived from ligands containing N-oxide units
;
_journal_issue                   1
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              115
_journal_paper_doi               10.1039/b711039a
_journal_volume                  32
_journal_year                    2008
_chemical_formula_sum            'C65 H47 Cd2 Cl4 N17 O24 S4'
_chemical_formula_weight         1945.04
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                93.2420(10)
_cell_angle_beta                 99.9830(10)
_cell_angle_gamma                97.9550(10)
_cell_formula_units_Z            2
_cell_length_a                   11.4892(8)
_cell_length_b                   13.6419(9)
_cell_length_c                   23.7577(16)
_cell_measurement_reflns_used    8475
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      48.302
_cell_measurement_theta_min      4.369
_cell_volume                     3619.6(4)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SHELXTL (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2001)'
_computing_publication_material  'SHELXTL (Bruker, 2001)'
_computing_structure_refinement  'SHELXTL (Bruker, 2001)'
_computing_structure_solution    'SHELXTL (Bruker, 2001)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 8.2
_diffrn_measured_fraction_theta_full 0.931
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'frames each covering 0.3\% in\w'
_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  0.0411
_diffrn_reflns_av_sigmaI/netI    0.0956
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            27891
_diffrn_reflns_theta_full        27.62
_diffrn_reflns_theta_max         27.62
_diffrn_reflns_theta_min         1.51
_exptl_absorpt_coefficient_mu    0.944
_exptl_absorpt_correction_T_max  0.843338
_exptl_absorpt_correction_T_min  0.653110
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.785
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.902
_refine_diff_density_min         -1.011
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.906
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1111
_refine_ls_number_reflns         15653
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      0.914
_refine_ls_R_factor_all          0.0975
_refine_ls_R_factor_gt           0.0439
_refine_ls_shift/su_max          0.038
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0525P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0927
_refine_ls_wR_factor_ref         0.1101
_reflns_number_gt                9053
_reflns_number_total             15653
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b711039a.txt
_cod_data_source_block           craigzm
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7051803