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_7012085
_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         '(C44 H46 N2 P2 Zn1).1/4(C7 H8)'
_chemical_formula_sum            'C45.75 H48 N2 P2 Zn'
_chemical_formula_weight         753.17
_chemical_name_common            '[ZnMe{MesNPPh2CHPPh2NMes}].0.25toluene'
_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/cifdics/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1
_audit_creation_date             2001-11-27T12:01:23-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                112.223(2)
_cell_angle_beta                 95.261(4)
_cell_angle_gamma                92.019(4)
_cell_formula_units_Z            4
_cell_length_a                   11.2619(5)
_cell_length_b                   18.4588(13)
_cell_length_c                   20.2548(13)
_cell_measurement_reflns_used    11282
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      21.967
_cell_measurement_theta_min      4.076
_cell_measurement_wavelength     0.71073
_cell_volume                     3870.2(4)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_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 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       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  0.1039
_diffrn_reflns_av_unetI/netI     0.1259
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            20269
_diffrn_reflns_theta_full        21.98
_diffrn_reflns_theta_max         21.98
_diffrn_reflns_theta_min         4.1
_exptl_absorpt_coefficient_mu    0.752
_exptl_absorpt_correction_T_max  0.986
_exptl_absorpt_correction_T_min  0.917
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
(see. N.W. Alcock (1970). Cryst. Computing, p271)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1586
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.659
_refine_diff_density_min         -0.469
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     913
_refine_ls_number_reflns         9360
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1099
_refine_ls_R_factor_gt           0.0654
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0190P)^2^+8.8441P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1237
_refine_ls_wR_factor_ref         0.1411
_reflns_number_gt                6313
_reflns_number_total             9360
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b207358g.txt
_cod_data_source_block           msh3-(nov1501)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7012085