DACH-Bridged (DACH =trans-1,2-Diaminocyclohexane) Bis(iminophosphonamide) Derivatives of Groups 3 and 13 and Their Use in the Enantiomorphic Polymerization of Methyl Methacrylate
Ahmed, Shabana A.; Hill, Michael S.; Hitchcock, Peter B.; Mansell, Stephen M.; St John, Oliver; Organometallics 26 (2007) 538–; doi:10.1021/om060860+

data_4083648
_publ_section_title
;
 DACH-Bridged (DACH =trans-1,2-Diaminocyclohexane) Bis(iminophosphonamide)
 Derivatives of Groups 3 and 13 and Their Use in the Enantiomorphic
 Polymerization of Methyl Methacrylate
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              538
_journal_paper_doi               10.1021/om060860+
_journal_volume                  26
_journal_year                    2007
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C46 H50 N4 P2'
_chemical_formula_sum            'C46 H50 N4 P2'
_chemical_formula_weight         720.84
_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      2.3
_audit_creation_date             2005-05-12T15:12:37-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 106.376(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.7450(3)
_cell_length_b                   19.6556(6)
_cell_length_c                   17.8171(6)
_cell_measurement_reflns_used    16821
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.022
_cell_measurement_theta_min      3.395
_cell_measurement_wavelength     0.71073
_cell_volume                     3946.3(2)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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      -0.410006E-1
_diffrn_orient_matrix_UB_12      -0.74886E-2
_diffrn_orient_matrix_UB_13      -0.56706E-1
_diffrn_orient_matrix_UB_21      -0.626966E-1
_diffrn_orient_matrix_UB_22      -0.272193E-1
_diffrn_orient_matrix_UB_23      0.143494E-1
_diffrn_orient_matrix_UB_31      -0.475745E-1
_diffrn_orient_matrix_UB_32      0.42325E-1
_diffrn_orient_matrix_UB_33      -0.805E-3
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0776
_diffrn_reflns_av_unetI/netI     0.0754
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            32094
_diffrn_reflns_theta_full        26.03
_diffrn_reflns_theta_max         26.03
_diffrn_reflns_theta_min         3.52
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.148
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.236
_refine_diff_density_min         -0.279
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         7753
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.1001
_refine_ls_R_factor_gt           0.0527
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0411P)^2^+1.6531P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0994
_refine_ls_wR_factor_ref         0.116
_reflns_number_gt                5079
_reflns_number_total             7753
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060860%2Bsi20060920_064345.cif
_cod_data_source_block           (2)-may805
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4083648