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_4318636
_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            'C42 H54 P2'
_chemical_formula_weight         620.79
_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                63.6983(6)
_cell_angle_beta                 80.3553(7)
_cell_angle_gamma                64.1540(5)
_cell_formula_units_Z            2
_cell_length_a                   12.2774(2)
_cell_length_b                   13.1536(2)
_cell_length_c                   14.4521(2)
_cell_measurement_reflns_used    6612
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.0
_cell_volume                     1882.03(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      173(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0448
_diffrn_reflns_av_sigmaI/netI    0.0443
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9076
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.84
_exptl_absorpt_coefficient_mu    0.142
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.095
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.551
_refine_diff_density_min         -0.406
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.947
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         4728
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.947
_refine_ls_R_factor_all          0.0843
_refine_ls_R_factor_gt           0.0706
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1977
_refine_ls_wR_factor_ref         0.2113
_reflns_number_gt                4040
_reflns_number_total             4728
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic025759l_s1_1.cif
_cod_data_source_block           pro01r
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        1882.04(4)
_cod_database_code               4318636