The relative stabilities of cyclic dicationic derivatives of diphosphanes with three (3P) or four (4P) linked phosphorus atoms.
Bashforth, Rachel; Boyall, Alice J.; Coffer, Philippa K.; Dillon, Keith B.; Goeta, Andrés E; Howard, Judith A. K.; Kenwright, Alan M.; Probert, Michael R.; Shepherd, Helena J.; Thompson, Amber L.; Dalton transactions (Cambridge, England : 2003) 41 (2012) 1165–1172; doi:10.1039/c1dt11549a

data_7017851
_publ_section_title
;
 The relative stabilities of cyclic dicationic derivatives of diphosphanes
 with three (3P) or four (4P) linked phosphorus atoms.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1165
_journal_page_last               1172
_journal_paper_doi               10.1039/c1dt11549a
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety
'2(C39 H59 P3), Cl6 Sn, 7.982(C H Cl3), 2(Cl3 Sn)'
_chemical_formula_sum            'C85.982 H125.982 Cl35.946 P6 Sn3'
_chemical_formula_weight         2975.87
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                72.928(2)
_cell_angle_beta                 87.477(2)
_cell_angle_gamma                72.386(2)
_cell_formula_units_Z            1
_cell_length_a                   10.5087(6)
_cell_length_b                   15.1261(8)
_cell_length_c                   20.8450(10)
_cell_measurement_reflns_used    4030
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      24.914
_cell_measurement_theta_min      2.233
_cell_volume                     3015.3(3)
_computing_data_collection       'SMART v5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics
;
Olex2, Durham University (compiled Feb 15 2009 13:03:59)
;
_computing_publication_material
;
Olex2, Durham University (compiled Feb 15 2009 13:03:59)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 8.0
_diffrn_detector_type            'Bruker SMART CCD 1K area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 1K area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.081221
_diffrn_orient_matrix_UB_12      0.022212
_diffrn_orient_matrix_UB_13      -0.005989
_diffrn_orient_matrix_UB_21      0.010465
_diffrn_orient_matrix_UB_22      -0.011287
_diffrn_orient_matrix_UB_23      -0.045044
_diffrn_orient_matrix_UB_31      -0.056988
_diffrn_orient_matrix_UB_32      0.068133
_diffrn_orient_matrix_UB_33      -0.021247
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0894
_diffrn_reflns_av_sigmaI/netI    0.1089
_diffrn_refln_scan_width         0.3
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            35805
_diffrn_reflns_theta_full        26.42
_diffrn_reflns_theta_max         26.42
_diffrn_reflns_theta_min         1.02
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           35.0
_diffrn_source_power             1.75
_diffrn_source_target            Mo
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.534
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.771354
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.638
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1490
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.415
_refine_diff_density_min         -0.947
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     607
_refine_ls_number_reflns         12391
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.1113
_refine_ls_R_factor_gt           0.0520
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
calc w=1/[\s^2^(Fo^2^)+(0.0569P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1090
_refine_ls_wR_factor_ref         0.1301
_reflns_number_gt                7439
_reflns_number_total             12391
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt11549a.txt
_cod_data_source_block           6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               7017851