Coordination Chemistry of Isomeric Mixtures of Linked Di(phosphaguanidine) Compounds: A Spectroscopic and Crystallographic Study
Mansfield, Natalie E.; Coles, Martyn P.; Avent, Anthony G.; Hitchcock, Peter B.; Organometallics 25 (2006) 2470–; doi:10.1021/om060014z

data_4075057
_publ_section_title
;
 Coordination Chemistry of Isomeric Mixtures of Linked
 Di(phosphaguanidine) Compounds:&#x00A0; A Spectroscopic and
 Crystallographic Study
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              2470
_journal_paper_doi               10.1021/om060014z
_journal_volume                  25
_journal_year                    2006
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C32 H54 Al2 N4 P2'
_chemical_formula_sum            'C32 H54 Al2 N4 P2'
_chemical_formula_weight         610.69
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_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      2.3
_audit_creation_date             2005-07-20T11:41:50-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                107.397(2)
_cell_angle_beta                 93.777(3)
_cell_angle_gamma                102.148(3)
_cell_formula_units_Z            1
_cell_length_a                   8.0203(3)
_cell_length_b                   9.6862(5)
_cell_length_c                   13.3190(6)
_cell_measurement_reflns_used    9431
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.022
_cell_measurement_theta_min      3.395
_cell_measurement_wavelength     0.71073
_cell_volume                     956.02(8)
_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-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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      -0.72811E-1
_diffrn_orient_matrix_UB_12      0.450593E-1
_diffrn_orient_matrix_UB_13      0.525596E-1
_diffrn_orient_matrix_UB_21      0.572668E-1
_diffrn_orient_matrix_UB_22      -0.328972E-1
_diffrn_orient_matrix_UB_23      0.547186E-1
_diffrn_orient_matrix_UB_31      0.894515E-1
_diffrn_orient_matrix_UB_32      0.96532E-1
_diffrn_orient_matrix_UB_33      0.235411E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0703
_diffrn_reflns_av_unetI/netI     0.0579
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14114
_diffrn_reflns_theta_full        25.95
_diffrn_reflns_theta_max         25.95
_diffrn_reflns_theta_min         3.6
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.184
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.061
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             330
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.523
_refine_diff_density_min         -0.384
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.76
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     180
_refine_ls_number_reflns         3707
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.76
_refine_ls_R_factor_all          0.0885
_refine_ls_R_factor_gt           0.0584
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1426P)^2^+1.9406P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1617
_refine_ls_wR_factor_ref         0.1944
_reflns_number_gt                2723
_reflns_number_total             3707
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060014zsi20060105_063055.cif
_cod_data_source_block           (2a-meso)-jul1805
_cod_original_cell_volume        956.02(7)
_cod_database_code               4075057