Synthesis and Structure of Mercurous Ion and Dinuclear Lead(II) Complexes of the 28-Membered Selenaaza Macrocycle: Dominance of the Chelate Ring Size Effect and Conformational Requirement over Soft-Soft Interactions
Snigdha Panda; Harkesh B. Singh; Ray J. Butcher; Inorganic Chemistry 43 (2004) 8532–8537; doi:10.1021/ic0351949

data_4312193
_publ_section_title
;
 Synthesis and Structure of Mercurous Ion and Dinuclear Lead(II) Complexes
 of the 28-Membered Selenaaza Macrocycle: Dominance of the Chelate Ring
 Size Effect and Conformational Requirement over Soft-Soft Interactions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8532
_journal_page_last               8537
_journal_paper_doi               10.1021/ic0351949
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C30 H24 F12 N2 O2 P2 Pd Se2'
_chemical_formula_weight         998.77
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           92
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.7737(10)
_cell_length_b                   10.7737(10)
_cell_length_c                   28.190(5)
_cell_measurement_temperature    293(2)
_cell_volume                     3272.1(7)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0688
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            2677
_diffrn_reflns_theta_max         29.99
_diffrn_reflns_theta_min         2.67
_exptl_absorpt_coefficient_mu    2.993
_exptl_crystal_density_diffrn    2.027
_exptl_crystal_F_000             1944
_refine_diff_density_max         0.728
_refine_diff_density_min         -0.646
_refine_diff_density_rms         0.114
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(3)
_refine_ls_extinction_coef       0.00017(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.039
_refine_ls_goodness_of_fit_obs   1.074
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         2677
_refine_ls_number_restraints     64
_refine_ls_restrained_S_all      1.028
_refine_ls_restrained_S_obs      1.056
_refine_ls_R_factor_all          0.0890
_refine_ls_R_factor_obs          0.0499
_refine_ls_shift/esd_max         1.069
_refine_ls_shift/esd_mean        0.057
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0034P)^2^+10.6286P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1006
_refine_ls_wR_factor_obs         0.0837
_reflns_number_observed          1858
_reflns_number_total             2677
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0351949rom20031016_064230_2.cif
_cod_data_source_block           hydrolysed_Pd(II)_complex_of_7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0034P)^2^+10.6286P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0034P)^2^+10.6286P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4312193