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_4323361
_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     'C45 H37 Br2 Hg O P3 - 2 C H2 Cl2'
_chemical_formula_sum            'C47 H41 Br2 Cl4 Hg O P3'
_chemical_formula_weight         1216.92
_chemical_name_systematic
;
 Dibromo-(2-methoxy-1,3-bis(triphenylphosphonio)-isophosphindol)-
 quecksilber(II)
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 91.910(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.028(2)
_cell_length_b                   15.513(2)
_cell_length_c                   30.247(8)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    208(2)
_cell_measurement_theta_max      46
_cell_measurement_theta_min      40
_cell_volume                     9392(3)
_computing_cell_refinement       'Enraf-Nonius CAD4'
_computing_data_collection       'Enraf-Nonius CAD4'
_computing_data_reduction        'XCAD4 (Sheldrick & Harms, 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      208(2)
_diffrn_measurement_device       'Enraf-Nonius CAD4'
_diffrn_measurement_method       two-theta/omega-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuKa
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0596
_diffrn_reflns_av_sigmaI/netI    0.0363
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            8123
_diffrn_reflns_theta_max         64.85
_diffrn_reflns_theta_min         2.92
_diffrn_standards_decay_%        +-3
_diffrn_standards_interval_count '200 (orientation)'
_diffrn_standards_interval_time  '120 (intensity)'
_diffrn_standards_number         '2 (orientation), 3 (intensity)'
_exptl_absorpt_coefficient_mu    11.205
_exptl_absorpt_correction_type   DIFABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.721
_exptl_crystal_description       prisms
_exptl_crystal_F_000             4752
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.595
_refine_diff_density_min         -3.454
_refine_diff_density_rms         .212
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.115
_refine_ls_goodness_of_fit_obs   1.145
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         7955
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.115
_refine_ls_restrained_S_obs      1.145
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_obs          0.0568
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s^2^(Fo^2^)+( 0.1193P)^2^+57.8497P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1774
_refine_ls_wR_factor_obs         0.1648
_reflns_number_observed          6593
_reflns_number_total             7955
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic960883o_2.cif
_cod_data_source_block           ms02ttda
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[s^2^(Fo^2^)+(
0.1193P)^2^+57.8497P] 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^)+( 0.1193P)^2^+57.8497P]
where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        9392.4(29)
_cod_database_code               4323361