P-Amino-cyclopentadienylidene-phosphoranes versus P-cyclopentadienyl-iminophosphoranes—tautomeric protic forms of a new bidentate CpPN ligand system
Petrov, Alex R.; Rufanov, Konstantin A.; Ziemer, Burkhard; Neubauer, Petra; Kotov, Vasily V.; Sundermeyer, Jörg; Dalton Transactions  (2008) 909–915; doi:10.1039/b710419g

data_7003056
_publ_section_title
;
 P-Amino-cyclopentadienylidene-phosphoranes versus
 P-cyclopentadienyl-iminophosphoranes---tautomeric protic forms of a
 new bidentate CpPN ligand system
;
_journal_issue                   7
_journal_name_full               'Dalton Transactions'
_journal_page_first              909
_journal_page_last               915
_journal_paper_doi               10.1039/b710419g
_journal_year                    2008
_chemical_formula_moiety         'C29 H32 N P'
_chemical_formula_sum            'C29 H32 N P'
_chemical_formula_weight         425.53
_chemical_name_common
;P-(N-2,6-diisopropylanilino)-cyclopentadienylidene-
diphenylphosphorane
;
_chemical_name_systematic
;
P-(N-2,6-diisopropylanilino)-cyclopentadienylidene-
diphenylphosphorane
;
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.73(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.781(2)
_cell_length_b                   23.416(2)
_cell_length_c                   10.692(3)
_cell_measurement_reflns_used    3000
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.5
_cell_volume                     2413.6(9)
_computing_cell_refinement       'IPDS2.87 (Stoe & Cie, 1997)'
_computing_data_collection       'IPDS2.87 (Stoe & Cie, 1997)'
_computing_data_reduction        'IPDS2.87 (Stoe & Cie, 1997)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean 6.667
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device       'Stoe IPDS diffractometer'
_diffrn_measurement_method       '\f-oscill.,\f-incr.=1.4\%,174 exposures'
_diffrn_radiation_monochromator  'planar graphite'
_diffrn_radiation_source         'fine-focus sealed X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0673
_diffrn_reflns_av_sigmaI/netI    0.0483
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            16846
_diffrn_reflns_theta_full        25.93
_diffrn_reflns_theta_max         25.93
_diffrn_reflns_theta_min         2.28
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.130
_exptl_absorpt_correction_T_max  0.9597
_exptl_absorpt_correction_T_min  0.9033
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
The correction was carried out by ABSCOR (Stoe, 1997), a modification of
DIFABS (Walker, N. & Stuart, D. (1983). Acta Cryst. A39, 158-166.
In contrary to DIFABS, ABSCOR loads F^2^ values instead of F ones.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.171
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.80
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.304
_refine_diff_density_min         -0.287
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         4597
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0396
_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^)+(0.0695P)^2^+0.0426P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1016
_refine_ls_wR_factor_ref         0.1065
_reflns_number_gt                3757
_reflns_number_total             4597
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            b710419g.txt
_cod_data_source_block           ruf18
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7003056