New homoleptic bis(pyrrolylpyridiylimino) Mg(II) and Zn(II) complexes as catalysts for the ring opening polymerization of cyclic esters via an "activated monomer" mechanism.
D'Auria, Ilaria; Tedesco, Consiglia; MAZZEO, Mina; Pellecchia, Claudio; Dalton Trans.  (2017) –; doi:10.1039/C7DT02445B

data_7043991
_publ_section_title
;
 New homoleptic bis(pyrrolylpyridiylimino) Mg(II) and Zn(II) complexes as
 catalysts for the ring opening polymerization of cyclic esters via an
 "activated monomer" mechanism.
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02445B
_journal_year                    2017
_chemical_formula_moiety         '2(C44 H48 Mg N6), 3(C7 H8)'
_chemical_formula_sum            'C109 H120 Mg2 N12'
_chemical_formula_weight         1646.78
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-03-25
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2017-06-08 deposited with the CCDC.
2017-08-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.462(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   18.885(4)
_cell_length_b                   12.5765(19)
_cell_length_c                   21.644(4)
_cell_measurement_reflns_used    11469
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.3637
_cell_measurement_theta_min      1.1942
_cell_volume                     4641.3(15)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device
;
Mercury2 (2x2 bin mode)
;
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_source         'Sealed Tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1068
_diffrn_reflns_av_unetI/netI     0.1664
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            37826
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.640
_diffrn_reflns_theta_min         1.926
_exptl_absorpt_coefficient_mu    0.082
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7809
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_description       prism
_exptl_crystal_F_000             1764
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene'
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.605
_refine_diff_density_min         -0.317
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     546
_refine_ls_number_reflns         11395
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.1845
_refine_ls_R_factor_gt           0.0864
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0678P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1784
_refine_ls_wR_factor_ref         0.2189
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5486
_reflns_number_total             11395
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02445b2.cif
_cod_data_source_block           new4_ct
_cod_original_cell_volume        4641.3(14)
_cod_database_code               7043991
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: C52(0.5) H52A(0.5) H52B(0.5) H52C(0.5) C53(0.5) C58(0.5) H58(0.5)
 C57(0.5) H57(0.5) C56(0.5) H56(0.5) C55(0.5) H55(0.5) C54(0.5) H54(0.5)
3.a Free rotating group:
 C52(C53,C58,C57,C56,C55,C54)
3.b Ternary CH refined with riding coordinates:
 C17(H17), C20(H20), C39(H39), C42(H42)
3.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C6(H6), C7(H7), C8(H8), C10(H10), C13(H13), C14(H14),
 C15(H15), C23(H23), C24(H24), C25(H25), C28(H28), C29(H29), C30(H30), C32(H32),
  C35(H35), C36(H36), C37(H37), C46(H46), C47(H47), C48(H48), C49(H49),
 C50(H50), C58(H58), C57(H57), C56(H56), C55(H55), C54(H54)
3.d Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C43(H43A,H43B,H43C), C44(H44A,
 H44B,H44C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C)
;
_shelx_res_checksum              89715
_olex2_submission_special_instructions 'No special instructions were received'