Syntheses and Structural Characterizations of the Unsymmetrical Diphosphene DmpPPMes* (Dmp = 2,6-Mes2C6H3, Mes* = 2,4,6-tBu3C6H2) and the Cyclotetraphosphane [DmpPPPh]2
Rhett C. Smith; Eugenijus Urnezius; Kin-Chung Lam; Arnold L. Rheingold; John D. Protasiewicz; Inorganic Chemistry 41 (2002) 5296–5299; doi:10.1021/ic025759l

data_4318637
_publ_section_title
;
 Syntheses and Structural Characterizations of the Unsymmetrical
 Diphosphene DmpPPMes* (Dmp = 2,6-Mes2C6H3, Mes* = 2,4,6-tBu3C6H2) and the
 Cyclotetraphosphane [DmpPPPh]2
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5296
_journal_page_last               5299
_journal_paper_doi               10.1021/ic025759l
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C62 H64 O0.5 P4'
_chemical_formula_weight         941.01
_chemical_melting_point          ?
_chemical_name_common
1,3-bis(2,6-dimesitylphenyl)-2,4-diphenylcyclotetraphosphane
_chemical_name_systematic
; 
 ? 
;
_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                80.933(8)
_cell_angle_beta                 78.112(7)
_cell_angle_gamma                62.186(6)
_cell_formula_units_Z            2
_cell_length_a                   12.4811(13)
_cell_length_b                   13.0376(13)
_cell_length_c                   19.996(2)
_cell_measurement_reflns_used    8782
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.50
_cell_measurement_theta_min      1.99
_cell_volume                     2809.1(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0423
_diffrn_reflns_av_sigmaI/netI    0.1099
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            10151
_diffrn_reflns_theta_full        24.00
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    0.172
_exptl_absorpt_correction_type   'psi scans'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.113
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'hexagonal prism'
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.555
_refine_diff_density_min         -0.264
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     599
_refine_ls_number_reflns         8782
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.1504
_refine_ls_R_factor_gt           0.0770
_refine_ls_shift/su_max          0.102
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1187P)^2^+1.0076P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2072
_refine_ls_wR_factor_ref         0.2450
_reflns_number_gt                4941
_reflns_number_total             8782
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic025759l_s1_2.cif
_cod_data_source_block           ring10
_cod_depositor_comments
;
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 1569 2011-02-09 13:29:24Z 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_original_cell_volume        2809.0(5)
_cod_original_formula_sum        'C62 H64 O0.50 P4'
_cod_database_code               4318637