Synthesis and structure of [{Sn(μ‒PCy)}3(Na·PMDETA)2], containing an electron-deficient [{Sn(μ‒PCy)}3]2- dianion
Alvarez-Bercedo, Paula; Bond, Andrew D.; Haigh, Robert; Hopkins, Alexander D.; Lawson, Gavin T.; McPartlin, Mary; Moncrieff, David; Gonzalez Mosquera, Marta E.; Rawson, Jeremy M.; Woods, Anthony D.; Wright, Dominic S.; Chemical Communications (Cambridge, United Kingdom)  (2003) 1288–1289; doi:10.1039/b300522d

data_7103664
_publ_section_title
;
 Synthesis and structure of [{Sn(\m--PCy)}3(Na&#x00B7;PMDETA)2],
 containing an electron-deficient [{Sn(\m--PCy)}3]2- dianion
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   11
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              1288
_journal_page_last               1289
_journal_paper_doi               10.1039/b300522d
_journal_year                    2003
_chemical_formula_sum            'C50 H95 N6 Na2 P3 Sn3'
_chemical_formula_weight         1275.28
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.7610(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.3877(2)
_cell_length_b                   13.2005(2)
_cell_length_c                   26.5244(4)
_cell_measurement_reflns_used    52478
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      1.00
_cell_volume                     6388.56(15)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius B.V. 1998)'
_computing_data_reduction
;
HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_publication_material  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_solution    'SIR-92 (Altomare et al. 1994)'
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'Thin slice \w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_av_sigmaI/netI    0.0440
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            38602
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.61
_exptl_absorpt_coefficient_mu    1.286
_exptl_absorpt_correction_T_max  0.845
_exptl_absorpt_correction_T_min  0.733
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
Sortav (Blessing 1995)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2616
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.942
_refine_diff_density_min         -0.677
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     737
_refine_ls_number_reflns         14519
_refine_ls_number_restraints     150
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0345
_refine_ls_shift/su_max          0.044
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0261P)^2^+5.8762P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0731
_refine_ls_wR_factor_ref         0.0801
_reflns_number_gt                11290
_reflns_number_total             14519
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b300522d.txt
_cod_data_source_block           mw0226
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7103664