Group 4 metal complexes of Trost's semi-crown ligand: synthesis, structural characterization and studies on the ring-opening polymerization of lactides and ε-caprolactone.
Rajashekhar, Bijja; Roymuhury, Sagnik K.; Chakraborty, Debashis; Ramkumar, Venkatachalam; Dalton transactions (Cambridge, England : 2003) 44 (2015) 16280–16293; doi:10.1039/c5dt02267c

data_7035978
_publ_section_title
;
 Group 4 metal complexes of Trost's semi-crown ligand: synthesis,
 structural characterization and studies on the ring-opening
 polymerization of lactides and \e-caprolactone.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16280
_journal_page_last               16293
_journal_paper_doi               10.1039/c5dt02267c
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C129 H132 N6 O12 Ti3, 3(C7 H8)'
_chemical_formula_sum            'C150 H156 N6 O12 Ti3'
_chemical_formula_weight         2378.50
_chemical_name_systematic        Ti
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-07-21 deposited with the CCDC.
2015-07-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.172(3)
_cell_length_b                   22.272(3)
_cell_length_c                   30.035(4)
_cell_measurement_reflns_used    3947
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      16.70
_cell_measurement_theta_min      2.29
_cell_volume                     12825(3)
_computing_cell_refinement       'Bruker APEXII'
_computing_data_collection       'Bruker APEXII'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1188
_diffrn_reflns_av_unetI/netI     0.0929
_diffrn_reflns_laue_measured_fraction_full 0.989
_diffrn_reflns_laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            33748
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        17.856
_diffrn_reflns_theta_max         17.856
_diffrn_reflns_theta_min         1.260
_exptl_absorpt_coefficient_mu    0.247
_exptl_absorpt_correction_T_max  0.948
_exptl_absorpt_correction_T_min  0.919
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/5(Bruker AXS.Inc)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.232
_exptl_crystal_description       Block
_exptl_crystal_F_000             5040
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.220
_refine_diff_density_max         0.420
_refine_diff_density_min         -0.272
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details
; 
 Flack x determined using 2520 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1501
_refine_ls_number_reflns         8537
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0813
_refine_ls_R_factor_gt           0.0544
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.2500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1332
_refine_ls_wR_factor_ref         0.1619
_reflns_Friedel_coverage         0.802
_reflns_friedel_fraction_full    0.989
_reflns_friedel_fraction_max     0.989
_reflns_number_gt                6663
_reflns_number_total             8537
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt02267c2.cif
_cod_data_source_block           Ti
_cod_depositor_comments
'Adding full bibliography for 7035976--7035978.cif.'
_cod_database_code               7035978
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.919
_shelx_estimated_absorpt_t_max   0.948
_shelx_res_checksum              71792