Crystallographic characterisation of Ti(iv) piperazine complexes and their exploitation for the ring opening polymerisation of rac-lactide.
Hancock, Stuart L.; Mahon, Mary F.; Jones, Matthew D.; Dalton transactions (Cambridge, England : 2003) 40 (2011) 2033–2037; doi:10.1039/c0dt01542c

data_7015027
_publ_section_title
;
 Crystallographic characterisation of Ti(iv) piperazine complexes and
 their exploitation for the ring opening polymerisation of rac-lactide.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2033
_journal_page_last               2037
_journal_paper_doi               10.1039/c0dt01542c
_journal_volume                  40
_journal_year                    2011
_chemical_formula_sum            'C56 H103 N2 O8 Ti2'
_chemical_formula_weight         1028.20
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                69.6250(10)
_cell_angle_beta                 89.943(2)
_cell_angle_gamma                62.8660(10)
_cell_formula_units_Z            2
_cell_length_a                   14.2220(3)
_cell_length_b                   15.3740(4)
_cell_length_c                   17.4080(4)
_cell_measurement_reflns_used    41364
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.51
_cell_volume                     3118.09(14)
_computing_cell_refinement       'HKL Scalepack (Otwinski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'HKL Denzo & Scalepack (Otwinski & 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
;
SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. ,
Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R.
(1999) J. Appl. Cryst. 32, 115-119.
;
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'nonius kappa ccd'
_diffrn_measurement_method       ccd
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0624
_diffrn_reflns_av_sigmaI/netI    0.0554
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            53805
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.75
_exptl_absorpt_coefficient_mu    0.303
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.095
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1122
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.680
_refine_diff_density_min         -0.630
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     717
_refine_ls_number_reflns         14135
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0976
_refine_ls_R_factor_gt           0.0607
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0913P)^2^+2.5340P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1579
_refine_ls_wR_factor_ref         0.1847
_reflns_number_gt                9735
_reflns_number_total             14135
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0DT01542C.TXT
_cod_data_source_block           Ti2(8)(OiPr)6
_cod_original_cell_volume        3118.09(13)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7015027