Phosphaguanidines as Scaffolds for Multimetallic Complexes Containing Metal-Functionalized Phosphines
Joanna Grundy; Natalie E. Mansfield; Martyn P. Coles; Peter B. Hitchcock; Inorganic Chemistry 47 (2008) 2258–2260; doi:10.1021/ic7024457

data_4304860
_publ_section_title
;
Phosphaguanidines as Scaffolds for Multimetallic Complexes Containing
Metal-Functionalized Phosphines
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2258
_journal_page_last               2260
_journal_paper_doi               10.1021/ic7024457
_journal_volume                  47
_journal_year                    2008
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C38 H50 Br1 Cu1 N4 P2'
_chemical_formula_sum            'C38 H50 Br Cu N4 P2'
_chemical_formula_weight         768.21
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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             2003-04-10T15:03:07-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 97.210(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4275(1)
_cell_length_b                   17.1857(2)
_cell_length_c                   22.3749(3)
_cell_measurement_reflns_used    40599
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.705
_cell_measurement_wavelength     0.71073
_cell_volume                     3977.96(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-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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      -0.476092E-1
_diffrn_orient_matrix_UB_12      -0.480286E-1
_diffrn_orient_matrix_UB_13      0.95469E-2
_diffrn_orient_matrix_UB_21      0.82918E-1
_diffrn_orient_matrix_UB_22      -0.299063E-1
_diffrn_orient_matrix_UB_23      0.4567E-2
_diffrn_orient_matrix_UB_31      0.142138E-1
_diffrn_orient_matrix_UB_32      0.135905E-1
_diffrn_orient_matrix_UB_33      0.437885E-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  0.0543
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            49814
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.71
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    1.664
_exptl_absorpt_correction_T_max  0.8351
_exptl_absorpt_correction_T_min  0.754
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.283
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.739
_refine_diff_density_min         -0.688
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     423
_refine_ls_number_reflns         9060
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.059
_refine_ls_R_factor_gt           0.0384
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0263P)^2^+4.1266P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0733
_refine_ls_wR_factor_ref         0.0805
_reflns_number_gt                7135
_reflns_number_total             9060
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic7024457-file003_3.cif
_cod_data_source_block           (4)-apr1303
_cod_original_formula_sum        'C38 H50 Br1 Cu1 N4 P2'
_cod_database_code               4304860