Effects of metal co-ordination geometry on self-assembly: a dinuclear double helicate complex and a tetranuclear cage complex of a new bis-bidentate bridging ligand
Paul, Rowena L.; Couchman, Samantha M.; Jeffery, John C.; McCleverty, Jon A.; Reeves, Zoe R.; Ward, Michael D.; Journal of the Chemical Society, Dalton Transactions  (2000) 845–; doi:10.1039/a909702c

data_7009275
_publ_section_title
;
 Effects of metal co-ordination geometry on self-assembly: a dinuclear
 double helicate complex and a tetranuclear cage complex of a new
 bis-bidentate bridging ligand
;
_journal_issue                   6
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              845
_journal_paper_doi               10.1039/a909702c
_journal_year                    2000
_chemical_formula_sum            'C48 H36 B F4 N13 O5.5 Pd2'
_chemical_formula_weight         1182.51
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 120.314(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   35.916(11)
_cell_length_b                   14.059(4)
_cell_length_c                   26.247(7)
_cell_measurement_temperature    173(2)
_cell_volume                     11441(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Siemens SMART Area Detector'
_diffrn_measurement_method
'\w rotation with narrow frames (0.3 degrees)'
_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  0.1766
_diffrn_reflns_av_sigmaI/netI    0.1620
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            18410
_diffrn_reflns_theta_full        20.00
_diffrn_reflns_theta_max         20.00
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    0.695
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.80
_exptl_absorpt_correction_type   'Empirical, pseudo-azimuthal scan (SADABS)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             4736
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.583
_refine_diff_density_min         -1.766
_refine_diff_density_rms         0.245
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.439
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     350
_refine_ls_number_reflns         5338
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.433
_refine_ls_R_factor_all          0.2306
_refine_ls_R_factor_gt           0.1696
_refine_ls_shift/su_max          0.301
_refine_ls_shift/su_mean         0.011
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4155
_refine_ls_wR_factor_ref         0.4440
_reflns_number_gt                3188
_reflns_number_total             5338
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            a909702c.txt
_cod_data_source_block           mdw
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C48 H36 B F4 N13 O5.50 Pd2'
_cod_database_code               7009275