Syntheses and X-ray Structures of Novel Main Group Bis(dialkylamino)phosphinimides†
Schulz, S.; Raab, M.; Nieger, M.; Niecke, E.; Organometallics 19 (2000) 2616–; doi:10.1021/om000059e

data_4077480
_publ_section_title
;
 Syntheses and X-ray Structures of Novel Main Group
 Bis(dialkylamino)phosphinimides&#x2020;
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              2616
_journal_paper_doi               10.1021/om000059e
_journal_volume                  19
_journal_year                    2000
_chemical_formula_sum            'C52 H102 Al2 N6 P2'
_chemical_formula_weight         927.30
_chemical_name_systematic
; 
 ? 
;
_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                97.738(2)
_cell_angle_beta                 106.838(2)
_cell_angle_gamma                101.366(2)
_cell_formula_units_Z            1
_cell_length_a                   9.0387(2)
_cell_length_b                   11.3829(4)
_cell_length_c                   14.5238(5)
_cell_measurement_reflns_used    23935
_cell_measurement_temperature    123(2)
_cell_volume                     1372.61(8)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       Collect
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    XP
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius KappaCCD'
_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  0.0327
_diffrn_reflns_av_sigmaI/netI    0.0369
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20460
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.99
_exptl_absorpt_coefficient_mu    0.150
_exptl_absorpt_correction_T_max  '0.9925 (theor.)'
_exptl_absorpt_correction_T_min  '0.9706 (theor.)'
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.122
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.282
_refine_diff_density_min         -0.286
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         4825
_refine_ls_number_restraints     81
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0366
_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^)+(0.0467P)^2^+0.3013P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0921
_refine_ls_wR_factor_ref         0.0963
_reflns_number_gt                3926
_reflns_number_total             4825
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om000059e.cif
_cod_data_source_block           compound_4
_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_original_cell_volume        1372.61(7)
_cod_original_sg_symbol_H-M      'P-1 (No.2)'
_cod_database_code               4077480