Synthesis and M-Cγ Hemilability of Group 2 Bis(phosphinimino)methanides
Shabana A. Ahmed; Michael S. Hill; Peter B. Hitchcock; Organometallics 25 (2006) 394–402; doi:10.1021/om050811h

data_4063233
_publ_section_title
;
 Synthesis and M-C\g Hemilability of Group 2
 Bis(phosphinimino)methanides
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              394
_journal_page_last               402
_journal_paper_doi               10.1021/om050811h
_journal_volume                  25
_journal_year                    2006
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C86 H86 K2 N4 P4, 3(C7 H8)'
_chemical_formula_sum            'C107 H110 K2 N4 P4'
_chemical_formula_weight         1654.07
_chemical_name_common
;
[{K(MesNPPh2CHPPh2NMes)}2]. 3(toluene)
;
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2003-09-08T15:31:21-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                100.458(1)
_cell_angle_beta                 94.304(1)
_cell_angle_gamma                119.129(1)
_cell_formula_units_Z            2
_cell_length_a                   14.4977(2)
_cell_length_b                   14.6883(2)
_cell_length_c                   25.7312(5)
_cell_measurement_reflns_used    49169
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      3.705
_cell_measurement_wavelength     0.71073
_cell_volume                     4620.91(13)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.802235E-1
_diffrn_orient_matrix_UB_12      -0.360553E-1
_diffrn_orient_matrix_UB_13      -0.75908E-2
_diffrn_orient_matrix_UB_21      -0.1029E-2
_diffrn_orient_matrix_UB_22      -0.238714E-1
_diffrn_orient_matrix_UB_23      -0.391007E-1
_diffrn_orient_matrix_UB_31      -0.57014E-2
_diffrn_orient_matrix_UB_32      -0.679027E-1
_diffrn_orient_matrix_UB_33      0.58294E-2
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0894
_diffrn_reflns_av_unetI/netI     0.0906
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            47014
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         3.71
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.221
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.189
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1756
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.07
_refine_diff_density_min         -0.719
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.185
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     956
_refine_ls_number_reflns         15913
_refine_ls_number_restraints     329
_refine_ls_restrained_S_all      1.173
_refine_ls_R_factor_all          0.2117
_refine_ls_R_factor_gt           0.1318
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0107P)^2^+45.3218P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2732
_refine_ls_wR_factor_ref         0.306
_reflns_number_gt                7829
_reflns_number_total             15913
_reflns_threshold_expression     >2sigma(I)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4063233