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_4312192
_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            'C32 H36 N4 Se2'
_chemical_formula_weight         634.57
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 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                 104.4830(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.3985(14)
_cell_length_b                   5.0714(4)
_cell_length_c                   18.2454(15)
_cell_measurement_temperature    293(2)
_cell_volume                     1469.1(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0437
_diffrn_reflns_av_sigmaI/netI    0.0662
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            10777
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         1.49
_exptl_absorpt_coefficient_mu    2.544
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.622573
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.88
_refine_diff_density_max         0.558
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.940
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         3581
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.940
_refine_ls_R_factor_all          0.0848
_refine_ls_R_factor_gt           0.0416
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0286P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0669
_refine_ls_wR_factor_ref         0.0739
_reflns_number_gt                2223
_reflns_number_total             3581
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0351949rom20031016_064230_1.cif
_cod_data_source_block           Compound_reduced_form_of_7
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_exptl_absorpt_correction_type' tag value 'multi-scans' was replaced
with 'multi-scan' value.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4312192