Synthesis, structure and reactivity of cyclopropenyl-1-ylidene stabilized S(II), Se(II) and Te(II) mono- and dications
Agnes Kozma; Jekaterina Petuskova; Christian W. Lehmann; Manuel Alcarazo; Chem.Commun. 49 (2013) 4145–; doi:10.1039/c2cc36225b

data_7109205
_publ_section_title
;
 Synthesis, structure and reactivity of cyclopropenyl-1-ylidene stabilized
 S(II), Se(II) and Te(II) mono- and dications
;
_journal_name_full               Chem.Commun.
_journal_page_first              4145
_journal_paper_doi               10.1039/c2cc36225b
_journal_volume                  49
_journal_year                    2013
_chemical_compound_source        dichloromethane,pentane
_chemical_formula_moiety         'C78.50 H92 B2 Cl F8 N4 P2 Pd2 Se2'
_chemical_formula_sum            'C78.5 H92 B2 Cl F8 N4 P2 Pd2 Se2'
_chemical_formula_weight         1733.29
_chemical_name_systematic
;
?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                KOZ-KA-091-02
_audit_creation_date             2012-04-05
_audit_creation_method
;
Olex2 1.1
(compiled 2011.11.01 svn.r2039, GUI svn.r3906)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 101.328(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.978(3)
_cell_length_b                   14.8026(18)
_cell_length_c                   28.165(3)
_cell_measurement_reflns_used    9840
_cell_measurement_temperature    100
_cell_measurement_theta_max      34.9295
_cell_measurement_theta_min      2.3712
_cell_volume                     8575.7(19)
_computing_cell_refinement       'SAINT software (Bruker AXS, 2004)'
_computing_data_collection       'APEX2 (Bruker AXS, 2008)'
_computing_data_reduction        'SAINT software (Bruker AXS, 2004)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact GbR, 2005)'
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-97 (G. M. Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (G. M. Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 66.67
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker-AXS Kappa Mach3 APEX-II'
_diffrn_measurement_method       'CCD \f- and \w-scans'
_diffrn_radiation_monochromator  'Incoatec Helios mirrors'
_diffrn_radiation_source         '0.2 x 2mm^2^ focus rotating anode'
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0562
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            306663
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         35.24
_diffrn_reflns_theta_min         0.99
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.395
_exptl_absorpt_correction_T_max  0.92978
_exptl_absorpt_correction_T_min  0.72404
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_description       plate
_exptl_crystal_F_000             3520
_exptl_crystal_size_max          0.222
_exptl_crystal_size_mid          0.211
_exptl_crystal_size_min          0.044
_platon_squeeze_details
;
Although there were four peaks within the void from Fourier difference map,
the highly disordered solvents within the void were not crystallographically
well defined.

The SQUEEZE routine suggested that a total potential solvent area volume of
720.4 Ang^3^ [ 8.4 % of cell volume] and a void electron population of
219 per cell.

Refinement after the SQUEEZE routine gave significantly improved R values.
[R values before SQUEEZE]
R1 =0.866 for > 4sigma(I) data
R1 = 0.1280, wR2 = 0.2959, GooF = S = 2.257 for all data
(38183 data and 0 restraint / 921 parameters)

Since a solvent mixture was used for crystallizing the compound the electron
density contained in the void was not interpreted chemically and the empirical
formula was not adjusted.
;
_refine_diff_density_max         3.363
_refine_diff_density_min         -1.192
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     920
_refine_ls_number_reflns         38183
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0484
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0849P)^2^+2.6507P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1384
_refine_ls_wR_factor_ref         0.1487
_reflns_number_gt                27463
_reflns_number_total             38183
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc36225b.txt
_cod_data_source_block           7765sadabs
_cod_original_cell_volume        8575.7(18)
_cod_original_sg_symbol_Hall     '-p 2ybc'
_cod_original_sg_symbol_H-M      P21/c
_cod_original_formula_sum        'C78.50 H92 B2 Cl F8 N4 P2 Pd2 Se2'
_cod_database_code               7109205