Reactions of Bis(triphenylphosphonio)isophosphindolide Salts with Mercury(II) Compounds: Coordination Induced Addition and Oxidation Reactions and Synthesis of a Monomeric 1:1 Complex of the Type [R2(R'O)P]HgBr2
Dietrich Gudat; Martin Nieger; Martin Schrott; Inorganic Chemistry 36 (1997) 1476–1481; doi:10.1021/ic960883o

data_4323360
_publ_section_title
;
 Reactions of Bis(triphenylphosphonio)isophosphindolide Salts with
 Mercury(II) Compounds: Coordination Induced Addition and Oxidation
 Reactions and Synthesis of a Monomeric 1:1 Complex of the Type
 [R2(R'O)P]HgBr2
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1476
_journal_page_last               1481
_journal_paper_doi               10.1021/ic960883o
_journal_volume                  36
_journal_year                    1997
_chemical_formula_analytical     'C44H34Cl5Hg2OP3 - 2 MeNO2'
_chemical_formula_sum            'C46 H42 Cl5 Hg2 N2 O5 P3'
_chemical_formula_weight         1374.16
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                   12.449(2)
_cell_length_b                   17.583(3)
_cell_length_c                   23.111(3)
_cell_measurement_reflns_used    50
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11.5
_cell_measurement_theta_min      10
_cell_volume                     5058.8(14)
_computing_cell_refinement       'P3 (Siemens, 1989)'
_computing_data_collection       'P3 (Siemens,1989)'
_computing_data_reduction        'SHELXTL-Plus (Sheldrick & Siemens, 1989)'
_computing_molecular_graphics    'SHELXTL-Plus (Sheldrick & Siemens, 1989)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXTL-Plus (Sheldrick & Siemens, 1989)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Nicolet R3m'
_diffrn_measurement_method       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  0.0558
_diffrn_reflns_av_sigmaI/netI    0.1038
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            9447
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.76
_diffrn_standards_decay_%        +-1.5
_diffrn_standards_interval_count 147
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.466
_exptl_absorpt_correction_T_max  0.955
_exptl_absorpt_correction_T_min  0.618
_exptl_absorpt_correction_type   'empirical with psi-scans'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.804
_exptl_crystal_description       prisms
_exptl_crystal_F_000             2648
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.913
_refine_diff_density_min         -0.717
_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   -0.009(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.889
_refine_ls_goodness_of_fit_obs   0.993
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     528
_refine_ls_number_reflns         8917
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.889
_refine_ls_restrained_S_obs      0.993
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_obs          0.0450
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0393P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1028
_refine_ls_wR_factor_obs         0.0970
_reflns_number_observed          6500
_reflns_number_total             8917
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic960883o_1.cif
_cod_data_source_block           ms06
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0393P)^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^)+(0.0393P)^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 
;
_cod_database_code               4323360