Synthesis, crystal and molecular structure of [Sn(η4-P2C2But2)]: the first non transition metal 1,3-diphosphacyclobutadienyl compound
Francis, Matthew D.; Hitchcock, Peter B.; Chemical Communications  (2002) 86–; doi:10.1039/b110228c

data_7114548
_publ_section_title
;
 Synthesis, crystal and molecular structure of [Sn(\h4-P2C2But2)]: the
 first non transition metal 1,3-diphosphacyclobutadienyl compound
;
_journal_issue                   1
_journal_name_full               'Chemical Communications'
_journal_page_first              86
_journal_paper_doi               10.1039/b110228c
_journal_year                    2002
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C10 H18 P2 Sn1'
_chemical_formula_sum            'C10 H18 P2 Sn'
_chemical_formula_weight         318.87
_chemical_name_common            '[Sn(P2(CtBu)2}]'
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_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_conform_dict_location     ftp://ftp.iucr.org/cifdics/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1
_audit_creation_date             2001-10-11T15:35:43-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 96.024(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.812(2)
_cell_length_b                   6.0863(8)
_cell_length_c                   10.6752(13)
_cell_measurement_reflns_used    4890
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      3.705
_cell_measurement_wavelength     0.71073
_cell_volume                     1280.1(3)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device       KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0571
_diffrn_reflns_av_unetI/netI     0.0568
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            2518
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         3.94
_exptl_absorpt_coefficient_mu    2.205
_exptl_absorpt_correction_T_max  0.831
_exptl_absorpt_correction_T_min  0.635
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.655
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.206
_refine_diff_density_min         -0.837
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     60
_refine_ls_number_reflns         1115
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0336
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0474P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0831
_refine_ls_wR_factor_ref         0.0859
_reflns_number_gt                998
_reflns_number_total             1115
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b110228c.txt
_cod_data_source_block           oct901
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7114548