Synthesis of C2 and Cs symmetric zinc complexes supported by bis(phosphinimino)methyl ligands and their use in ring opening polymerisation catalysis
Hill, Michael S.; Hitchcock, Peter B.; Journal of the Chemical Society, Dalton Transactions  (2002) 4694–; doi:10.1039/b207358g

data_7012086
_publ_section_title
;
 Synthesis of C2 and Cs symmetric zinc complexes supported by
 bis(phosphinimino)methyl ligands and their use in ring opening
 polymerisation catalysis
;
_journal_issue                   24
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4694
_journal_paper_doi               10.1039/b207358g
_journal_year                    2002
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         '(C41 H40 N2 P2 Zn1).1/2(C7 H8)'
_chemical_formula_sum            'C44.5 H44 N2 P2 Zn'
_chemical_formula_weight         734.13
_chemical_name_common
;
[Zn(Me)(MesNPPh2CHPPh2NPh)].1/2(toluene)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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             2002-05-08T09:44:44-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 98.4740(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.6605(3)
_cell_length_b                   14.7185(2)
_cell_length_c                   20.5047(2)
_cell_measurement_reflns_used    50380
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.682
_cell_measurement_theta_min      3.705
_cell_measurement_wavelength     0.71073
_cell_volume                     7659.75(16)
_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 0.938
_diffrn_measured_fraction_theta_max 0.938
_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  0.0623
_diffrn_reflns_av_unetI/netI     0.0522
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            61498
_diffrn_reflns_theta_full        25.66
_diffrn_reflns_theta_max         25.66
_diffrn_reflns_theta_min         3.71
_exptl_absorpt_coefficient_mu    0.758
_exptl_absorpt_correction_T_max  0.8441
_exptl_absorpt_correction_T_min  0.7898
_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    1.273
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3080
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.117
_refine_diff_density_min         -0.711
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     846
_refine_ls_number_reflns         13600
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0894
_refine_ls_R_factor_gt           0.0574
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0528P)^2^+18.8165P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1357
_refine_ls_wR_factor_ref         0.1524
_reflns_number_gt                9703
_reflns_number_total             13600
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b207358g.txt
_cod_data_source_block           msh4-(may602)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_original_formula_sum        'C44.50 H44 N2 P2 Zn'
_cod_database_code               7012086