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_7003422
_publ_section_title
;
 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_absolute_configuration unk
_chemical_formula_moiety         'C28 H29 P3, 2(Al Cl4)'
_chemical_formula_sum            'C28 H29 Al2 Cl8 P3'
_chemical_formula_weight         796.05
_chemical_melting_point          ?
_space_group_IT_number           32
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 -2ab'
_symmetry_space_group_name_H-M   'P b a 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             07-10-09
_audit_creation_method           CRYSTALS_ver_12.85
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.8830(16)
_cell_length_b                   31.806(2)
_cell_length_c                   9.8121(7)
_cell_measurement_reflns_used    5282
_cell_measurement_temperature    120
_cell_measurement_theta_max      27.470
_cell_measurement_theta_min      2.600
_cell_volume                     7141.4(8)
_computing_cell_refinement       'SMART-NT V6.1 (Bruker, 2000)'
_computing_data_collection       'SMART-NT V6.1 (Bruker, 2000)'
_computing_data_reduction        'SAINT-NT V6.45A (Bruker, 2000)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_device       'Bruker SMART'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.098
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            51876
_diffrn_reflns_theta_full        26.317
_diffrn_reflns_theta_max         28.298
_diffrn_reflns_theta_min         2.347
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.835
_exptl_absorpt_correction_T_max  0.9671
_exptl_absorpt_correction_T_min  0.8039
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian Integration (Busing and Levy, 1957)
;
_exptl_crystal_colour            clear_pale_colourless
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       block
_exptl_crystal_F_000             3232
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.72
_refine_diff_density_min         -0.79
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9473
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     741
_refine_ls_number_reflns         14723
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1058
_refine_ls_R_factor_gt           0.0695
_refine_ls_shift/su_max          0.000350
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.01P)^2^ +34.25P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1313
_refine_ls_wR_factor_gt          0.1120
_refine_ls_wR_factor_ref         0.1313
_reflns_limit_h_max              29
_reflns_limit_h_min              0
_reflns_limit_k_max              42
_reflns_limit_k_min              0
_reflns_limit_l_max              13
_reflns_limit_l_min              -12
_reflns_number_gt                10238
_reflns_number_total             15890
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.58
_oxford_diffrn_Wilson_scale      176.60
_oxford_refine_ls_r_factor_ref   0.1058
_oxford_refine_ls_scale          0.080761(12)
_oxford_reflns_number_all        14723
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            b716027e.txt
_cod_data_source_block           6c
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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 
;
_cod_database_code               7003422