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_7012087
_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         'C49 H61 N3 P2 Si2 Zn1'
_chemical_formula_sum            'C49 H61 N3 P2 Si2 Zn'
_chemical_formula_weight         875.5
_chemical_name_common            '[Zn{N(SiMe3)2}{MesNPPh2CHPPh2NMes}]'
_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             2002-03-22T16:45:07-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 100.1290
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2060(2)
_cell_length_b                   19.8779(4)
_cell_length_c                   19.7239(5)
_cell_measurement_reflns_used    18263
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.108
_cell_measurement_theta_min      3.705
_cell_measurement_wavelength     0.71073
_cell_volume                     4711.02(17)
_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 0.993
_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
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.339715E-1
_diffrn_orient_matrix_UB_12      0.415929E-1
_diffrn_orient_matrix_UB_13      -0.23321E-1
_diffrn_orient_matrix_UB_21      0.527641E-1
_diffrn_orient_matrix_UB_22      -0.24305E-2
_diffrn_orient_matrix_UB_23      -0.333889E-1
_diffrn_orient_matrix_UB_31      -0.546637E-1
_diffrn_orient_matrix_UB_32      -0.281945E-1
_diffrn_orient_matrix_UB_33      -0.315251E-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  0.0944
_diffrn_reflns_av_unetI/netI     0.0623
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            31199
_diffrn_reflns_theta_full        24.13
_diffrn_reflns_theta_max         24.13
_diffrn_reflns_theta_min         3.72
_exptl_absorpt_coefficient_mu    0.676
_exptl_absorpt_correction_T_max  0.8826
_exptl_absorpt_correction_T_min  0.8031
_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    1.234
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.927
_refine_diff_density_min         -0.472
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.12
_refine_ls_hydrogen_treatment    'riding; torsion refined for ortho-methyls'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     518
_refine_ls_number_reflns         7435
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.12
_refine_ls_R_factor_all          0.0895
_refine_ls_R_factor_gt           0.0654
_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^)+(0.0376P)^2^+17.9944P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1431
_refine_ls_wR_factor_ref         0.1549
_reflns_number_gt                5775
_reflns_number_total             7435
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b207358g.txt
_cod_data_source_block           msh5-(mar1502)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7012087