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_4075056
_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         'C40 H60 N4 P2'
_chemical_formula_sum            'C40 H60 N4 P2'
_chemical_formula_weight         658.86
_chemical_name_common            '[{-CH2P(Ph)C(NHcy)(Ncy)}2]'
_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      2.2
_audit_creation_date             2002-09-27T14:37:43-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                110.804(5)
_cell_angle_beta                 97.381(5)
_cell_angle_gamma                94.342(4)
_cell_formula_units_Z            1
_cell_length_a                   9.2204(7)
_cell_length_b                   10.0638(8)
_cell_length_c                   11.1221(9)
_cell_measurement_reflns_used    7908
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.722
_cell_measurement_theta_min      3.705
_cell_measurement_wavelength     0.71073
_cell_volume                     948.53(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_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0715
_diffrn_reflns_av_unetI/netI     0.0825
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5230
_diffrn_reflns_theta_full        22.89
_diffrn_reflns_theta_max         22.89
_diffrn_reflns_theta_min         3.98
_exptl_absorpt_coefficient_mu    0.147
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.153
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             358
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.258
_refine_diff_density_min         -0.217
_refine_diff_density_rms         0.047
_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     212
_refine_ls_number_reflns         2502
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0861
_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^)+(0.0421P)^2^+0.6512P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1227
_refine_ls_wR_factor_ref         0.1353
_reflns_number_gt                1910
_reflns_number_total             2502
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060014zsi20060105_063055.cif
_cod_data_source_block           (1b)-sep2202
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4075056