Highly Thermally Stable and Robust Enantiopure NNN-Scorpionate Zirconium Initiators for the Controlled Ring-Opening Polymerization of rac-Lactide
Otero, Antonio; fernandez, juan; garces, andres; SÁNCHEZ-BARBA MERLO, LUIS FERNANDO; lara, agustin; martinez-Ferrer, Jaime; Carrion, Maria Prado; Rodríguez, Ana María; Dalton Trans.  (2017) –; doi:10.1039/C7DT01050H

data_7042747
_publ_section_title
;
 Highly Thermally Stable and Robust Enantiopure NNN-Scorpionate Zirconium
 Initiators for the Controlled Ring-Opening Polymerization of rac-Lactide
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01050H
_journal_year                    2017
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C57 H71 F N5 S3 Zr, 0.5(C4 O)'
_chemical_formula_sum            'C59 H75 F N5 O0.5 S3 Zr'
_chemical_formula_weight         1068.64
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2017-04-18 deposited with the CCDC.
2017-04-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.641(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.9418(3)
_cell_length_b                   28.5201(8)
_cell_length_c                   10.9256(3)
_cell_measurement_reflns_used    1166
_cell_measurement_temperature    240(2)
_cell_measurement_theta_max      15.715
_cell_measurement_theta_min      2.217
_cell_volume                     3022.77(15)
_computing_cell_refinement       'Bruker SAINT V8.37 (Bruker AXS Inc. 2016)'
_computing_data_collection       'Bruker APEX'
_computing_data_reduction        'Bruker SAINT V8.37 (Bruker AXS Inc. 2016)'
_computing_molecular_graphics    'WINGX v2014.1 (Farrugia, 2012)'
_computing_publication_material  'WINGX v2014.1 (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      240(2)
_diffrn_measured_fraction_theta_full 0.933
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'CCD area detector, APEX'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1104
_diffrn_reflns_av_unetI/netI     0.2036
_diffrn_reflns_Laue_measured_fraction_full 0.933
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            15981
_diffrn_reflns_point_group_measured_fraction_full 0.935
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         1.428
_exptl_absorpt_coefficient_mu    0.328
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.607
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.174
_exptl_crystal_description       prism
_exptl_crystal_F_000             1130
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.542
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.10(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.957
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     656
_refine_ls_number_reflns         9418
_refine_ls_number_restraints     93
_refine_ls_restrained_S_all      0.956
_refine_ls_R_factor_all          0.1801
_refine_ls_R_factor_gt           0.0835
_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^)+(0.0935P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1764
_refine_ls_wR_factor_ref         0.2288
_reflns_Friedel_coverage         0.960
_reflns_Friedel_fraction_full    0.936
_reflns_Friedel_fraction_max     0.964
_reflns_number_gt                4585
_reflns_number_total             9418
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01050h2.cif
_cod_data_source_block           6
_cod_original_formula_sum        'C59 H75 F N5 O0.50 S3 Zr'
_cod_database_code               7042747
_shelx_estimated_absorpt_t_min   0.940
_shelx_estimated_absorpt_t_max   0.962
_shelxl_version_number           2013-4
_shelx_res_checksum              17113