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_7003055
_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         'C27 H30 N P'
_chemical_formula_sum            'C27 H30 N P'
_chemical_formula_weight         399.49
_chemical_name_common
;P-(N-Adamantyl-1-amino)-cyclopentadienylidene-
diphenylphosphorane
;
_chemical_name_systematic
;
P-(N-Adamantyl-1-amino)-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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.072(18)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.4180(16)
_cell_length_b                   9.7728(13)
_cell_length_c                   19.444(3)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      3.0
_cell_volume                     2142.5(5)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Stoe IPDS diffractometer'
_diffrn_measurement_method       '\f-oscill.,\f-incr.=1.3\%,176 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  0.0571
_diffrn_reflns_av_sigmaI/netI    0.0701
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            13689
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         2.56
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.142
_exptl_absorpt_correction_T_max  0.9668
_exptl_absorpt_correction_T_min  0.9561
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.291
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.041
_refine_ls_extinction_coef       0.0045(4)
_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_ref   0.860
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         3872
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.860
_refine_ls_R_factor_all          0.0637
_refine_ls_R_factor_gt           0.0343
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0307P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0647
_refine_ls_wR_factor_ref         0.0700
_reflns_number_gt                2567
_reflns_number_total             3872
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            b710419g.txt
_cod_data_source_block           ruf10
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7003055