Mononuclear Salen-gallium complexes for iso-selective ring-opening polymerization (ROP) of rac-lactide
SPECKLIN, David; Fliedel, Christophe; Hild, Frédéric; Mameri, Samir; Karmazin, Lydia; Bailly, Corinne; Dagorne, Samuel; Dalton Trans.  (2017) –; doi:10.1039/C7DT02730C

data_7044156
_publ_section_title
;
 Mononuclear Salen-gallium complexes for iso-selective ring-opening
 polymerization (ROP) of rac-lactide
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02730C
_journal_year                    2017
_chemical_formula_moiety         'C42 H59 Ga N2 O3, 1.5(C7 H8 O)'
_chemical_formula_sum            'C52.5 H71 Ga N2 O4.5'
_chemical_formula_weight         871.83
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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-2014/7
_audit_update_record
;
2017-09-06 deposited with the CCDC.
2017-09-08 downloaded from the CCDC.
;
_cell_angle_alpha                76.215(5)
_cell_angle_beta                 74.526(4)
_cell_angle_gamma                85.504(5)
_cell_formula_units_Z            2
_cell_length_a                   13.000(3)
_cell_length_b                   13.848(3)
_cell_length_c                   14.499(3)
_cell_measurement_reflns_used    6079
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.28
_cell_measurement_theta_min      2.36
_cell_volume                     2442.8(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_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    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1210
_diffrn_reflns_av_unetI/netI     0.1508
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            41138
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.331
_diffrn_reflns_theta_min         1.496
_diffrn_source                   'fine focus sealed tube'
_exptl_absorpt_coefficient_mu    0.609
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5610
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_description       block
_exptl_crystal_F_000             934
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.200
_platon_squeeze_details
;
 The residual electron density was assigned to half a molecule
 of the benzyl alcohol solvent  [54/2 = 27 e per asymmetric  
 unit; half a molecule of C7H8O would give 29e].
;
_refine_diff_density_max         0.641
_refine_diff_density_min         -1.237
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     519
_refine_ls_number_reflns         11750
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.1888
_refine_ls_R_factor_gt           0.0812
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1175P)^2^+3.2384P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2048
_refine_ls_wR_factor_ref         0.2651
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5758
_reflns_number_total             11750
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02730c2.cif
_cod_data_source_block           sdfh160802
_cod_original_formula_sum        'C52.50 H71 Ga N2 O4.50'
_cod_database_code               7044156
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.802
_shelx_estimated_absorpt_t_max   0.888
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              99198
_shelx_fab_checksum              52125