Persistent phosphinyl radicals from a bulky diphosphine: an example of a molecular jack-in-the-box
Hinchley, Sarah L.; Morrison, Carole A.; Rankin, David W. H.; Macdonald, Charles L. B.; Wiacek, Robert J.; Cowley, Alan H.; Lappert, Michael F.; Gundersen, Grete; Clyburne, Jason A. C.; Power, Philip P.; Chemical Communications  (2000) 2045–; doi:10.1039/b004889p

data_7115148
_publ_section_title
;
 Persistent phosphinyl radicals from a bulky diphosphine: an example of a
 molecular jack-in-the-box
;
_journal_issue                   20
_journal_name_full               'Chemical Communications'
_journal_page_first              2045
_journal_paper_doi               10.1039/b004889p
_journal_year                    2000
_chemical_compound_source        selfmade
_chemical_formula_analytical     n/a
_chemical_formula_moiety         'C28 H76 P2 Si8'
_chemical_formula_structural     '[((CH3)3Si)2)CH)2P]2 '
_chemical_formula_sum            'C28 H76 P2 Si8'
_chemical_formula_weight         699.55
_chemical_melting_point          ?
_chemical_name_common            tetra(disyl)diphosphine
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 110.650(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.341(2)
_cell_length_b                   13.4240(10)
_cell_length_c                   19.033(2)
_cell_measurement_reflns_used    55
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      12.49
_cell_measurement_theta_min      4.58
_cell_volume                     4385.0(8)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Siemens P4'
_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  0.0173
_diffrn_reflns_av_sigmaI/netI    0.0184
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -2
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            9263
_diffrn_reflns_theta_max         25.06
_diffrn_reflns_theta_min         1.19
_diffrn_standards_decay_%        7.85
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.335
_exptl_absorpt_correction_T_max  0.7984
_exptl_absorpt_correction_T_min  0.7332
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.060
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.295
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.055
_refine_ls_extinction_coef       0.0042(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.705
_refine_ls_goodness_of_fit_obs   1.783
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         7702
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.714
_refine_ls_restrained_S_obs      1.783
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_obs          0.0375
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0504P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1203
_refine_ls_wR_factor_obs         0.1159
_reflns_number_observed          6659
_reflns_number_total             7709
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b004889p.txt
_cod_data_source_block           final
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'n/a' was changed to '?' - the value
is undefined or not given.

'_symmetry_cell_setting' value
'Monoclinic' changed to 'monoclinic' according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' 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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0504P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0504P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4385.0(7)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7115148