Synthesis and Characterization of an Unsymmetrical 1,2-Diphosphinoethanide Complex
Förster, Daniela; Nieger, Martin; Gudat, Dietrich; Organometallics 30 (2011) 2628–; doi:10.1021/om200069t

data_4064372
_publ_section_title
;
 Synthesis and Characterization of an Unsymmetrical
 1,2-Diphosphinoethanide Complex
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2628
_journal_paper_doi               10.1021/om200069t
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C32 H34 N2 P2'
_chemical_formula_sum            'C32 H34 N2 P2'
_chemical_formula_weight         508.55
_chemical_name_systematic
; 
 1,3-Bis(2',6'-dimethylphenyl)-4,5-dimethyl-2-diphenylphosphino-
 [1,3,2]diazaphospholene 
;
_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                84.28(2)
_cell_angle_beta                 80.99(2)
_cell_angle_gamma                78.72(2)
_cell_formula_units_Z            2
_cell_length_a                   8.051(2)
_cell_length_b                   12.213(3)
_cell_length_c                   14.472(1)
_cell_measurement_reflns_used    96
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      1
_cell_volume                     1374.8(5)
_computing_cell_refinement       'DIRAX (Duisenberg, 1992)'
_computing_data_collection       'Collect (Nonius, 1998)'
_computing_data_reduction        'EVALCCD (Duisenberg, 2003)'
_computing_molecular_graphics    'XP Sheldrick'
_computing_publication_material  'SHELXL 97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Nonius-Bruker Kappa CCD'
_diffrn_measurement_method       'rotation in phi and omega, 2 deg.'
_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  0.0306
_diffrn_reflns_av_sigmaI/netI    0.0266
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            30636
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.14
_exptl_absorpt_coefficient_mu    0.182
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             540
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.340
_refine_diff_density_min         -0.236
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         6280
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0367
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0393P)^2^+0.7288P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0861
_refine_ls_wR_factor_ref         0.0933
_reflns_number_gt                5113
_reflns_number_total             6280
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200069t_si_001.cif
_cod_data_source_block           dg075_hy_daf02_compound_8
_cod_depositor_comments
;
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 
;
_cod_database_code               4064372