Lead complexation by novel phenanthroline-containing macrocycles †
Bazzicalupi, Carla; Bencini, Andrea; Fusi, Vieri; Giorgi, Claudia; Paoletti, Piero; Valtancoli, Barbara; Journal of the Chemical Society, Dalton Transactions  (1999) 393–; doi:10.1039/a806800c

data_7027101
_publ_section_title
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 Lead complexation by novel phenanthroline-containing
 macrocycles&#x200A;&#x2020;
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_journal_issue                   3
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              393
_journal_paper_doi               10.1039/a806800c
_journal_year                    1999
_chemical_formula_moiety
;
Pb 2+, C22 H31 N7, Cl O4 1-, B C24 H20 1-
;
_chemical_formula_structural
;
(Pb) (C22 H31 N7) (Cl O4) (B C24 H20)
;
_chemical_formula_sum            'C46 H51 B Cl N7 O4 Pb'
_chemical_formula_weight         1019.39
_chemical_name_systematic
;
 ?
;
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                89.16(7)
_cell_angle_beta                 84.90(10)
_cell_angle_gamma                71.90(10)
_cell_formula_units_Z            2
_cell_length_a                   9.777(7)
_cell_length_b                   13.700(10)
_cell_length_c                   16.750(10)
_cell_measurement_reflns_used    22
_cell_measurement_temperature    298
_cell_measurement_theta_max      11.2
_cell_measurement_theta_min      6.2
_cell_volume                     2124(3)
_computing_cell_refinement       'CAD4 Enraf-Nonius'
_computing_data_collection       'CAD4 Enraf-Nonius'
_computing_data_reduction        'CAD4 Enraf-Nonius'
_computing_molecular_graphics    'ORTEP (Johnson,1971)'
_computing_publication_material
;
SHELXL-93 (Sheldrick, 1993), PARST93 (Nardelli,1993)
;
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'patterson metod'
_diffrn_ambient_temperature      298
_diffrn_measurement_device       'CAD4 Enraf-Nonius'
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0611
_diffrn_reflns_av_sigmaI/netI    0.1580
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7724
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.61
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    4.088
_exptl_absorpt_correction_type   'refdelf (Walker and Stuart, 1983)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.594
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.822
_refine_diff_density_min         -3.084
_refine_diff_density_rms         0.217
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.026
_refine_ls_goodness_of_fit_obs   1.142
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         7443
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_restrained_S_obs      1.142
_refine_ls_R_factor_all          0.1910
_refine_ls_R_factor_obs          0.1031
_refine_ls_shift/esd_max         0.561
_refine_ls_shift/esd_mean        0.028
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1841P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3231
_refine_ls_wR_factor_obs         0.2519
_reflns_number_observed          3779
_reflns_number_total             7447
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            806800csup1.cif
_cod_data_source_block           '[PbL3](ClO4)(BPh4)'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1841P)^2^+0.0000P] 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^)+(0.1841P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_cell_volume        2123.9(25)
_cod_database_code               7027101