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_7109202
_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_absolute_configuration rmad
_chemical_compound_source        dichloromethane,ether
_chemical_formula_moiety         'C57 H63 N2 P2 Pt S, B F4'
_chemical_formula_sum            'C57 H63 B F4 N2 P2 Pt S'
_chemical_formula_weight         1151.99
_space_group_IT_number           14
_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-056-03
_audit_creation_date             2012-03-14
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.972(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.3202(18)
_cell_length_b                   15.5062(9)
_cell_length_c                   21.7660(16)
_cell_measurement_reflns_used    205222
_cell_measurement_temperature    100
_cell_measurement_theta_max      34.9999
_cell_measurement_theta_min      2.6173
_cell_volume                     5823.7(8)
_computing_cell_refinement       'DENZO (Bruker AXS, 2006)'
_computing_data_collection       'DATCOL (Bruker AXS, 2006)'
_computing_data_reduction        'DENZO (Bruker AXS, 2006)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact GbR, 2005)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 18.02
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker AXS Enraf-Nonius KappaCCD'
_diffrn_measurement_method       'CCD \f- and \w-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         '0.2 x 2mm^2^ focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0492
_diffrn_reflns_av_sigmaI/netI    0.0317
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            187089
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         34.97
_diffrn_reflns_theta_min         2.65
_exptl_absorpt_coefficient_mu    2.548
_exptl_absorpt_correction_T_max  0.65626
_exptl_absorpt_correction_T_min  0.45701
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_description       prism
_exptl_crystal_F_000             2336
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.09
_platon_squeeze_details
;
Although there were eight 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
803.5 Ang^3^ [ 13.7 % of cell volume] and a void electron population of
116 per cell.

Refinement after the SQUEEZE routine gave significantly improved R values.
[R values before SQUEEZE]
R1 = 0.0566 For >4sigma(I) data
R1 = 0.0764, wR2 = 0.1762, GooF = S = 1.094 for all data
(25515 data and 0 restraint / 598 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         2.237
_refine_diff_density_min         -1.510
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     597
_refine_ls_number_reflns         25535
_refine_ls_number_restraints     129
_refine_ls_restrained_S_all      1.186
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0428
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0511P)^2^+8.3349P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1081
_refine_ls_wR_factor_ref         0.1146
_reflns_number_gt                20849
_reflns_number_total             25535
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc36225b.txt
_cod_data_source_block           testsadabs
_cod_original_sg_symbol_Hall     '-p 2ybc'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7109202