Alkyl and aryl dicationic derivatives of cyclic triphosphenium ions
Dillon, Keith B.; Goeta, Andrés E.; Howard, Judith A. K.; Monks, Philippa K.; Shepherd, Helena J.; Thompson, Amber L.; Dalton Transactions  (2008) 1144–1149; doi:10.1039/b716027e

data_7003423
_publ_section_title
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 Alkyl and aryl dicationic derivatives of cyclic triphosphenium ions
;
_journal_issue                   9
_journal_name_full               'Dalton Transactions'
_journal_page_first              1144
_journal_page_last               1149
_journal_paper_doi               10.1039/b716027e
_journal_year                    2008
_chemical_formula_moiety         'C29 H31 P3, Cl6 Sn, 2(C H Cl3)'
_chemical_formula_sum            'C31 H33 Cl12 P3 Sn'
_chemical_formula_weight         1042.57
_chemical_melting_point          ?
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 94.6610(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.7862(8)
_cell_length_b                   21.2600(14)
_cell_length_c                   15.2904(10)
_cell_measurement_reflns_used    6891
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.892
_cell_measurement_theta_min      2.216
_cell_volume                     4142.7(5)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_collection       'SMART v5.630 (Bruker, 2003)'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART 1K CCD area detector'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0813
_diffrn_reflns_av_sigmaI/netI    0.0856
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            29989
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    1.531
_exptl_absorpt_correction_T_max  0.758
_exptl_absorpt_correction_T_min  0.574
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.0651 before and 0.0520 after correction.
The Ratio of minimum to maximum transmission is 0.758.
The \l/2 correction factor is 0.0000
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.672
_exptl_crystal_density_meas      ?
_exptl_crystal_description       Block
_exptl_crystal_F_000             2072
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.824
_refine_diff_density_min         -1.271
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         7314
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0969
_refine_ls_R_factor_gt           0.0671
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
calc w=1/[\s^2^(Fo^2^)+(0.0466P)^2^+27.8776P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1362
_refine_ls_wR_factor_ref         0.1460
_reflns_number_gt                5869
_reflns_number_total             8451
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b716027e.txt
_cod_data_source_block           6e
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
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_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7003423