High Performance Benzoimidazolyl-Based Aminophenolate Zinc Complexes for Isoselective Polymerization of rac-Lactide
Gong, Yanmei; Ma, Haiyan; Chemical Communications  (2019) –; doi:10.1039/C9CC04834K

data_7123921
_publ_section_title
;
 High Performance Benzoimidazolyl-Based Aminophenolate Zinc Complexes for
 Isoselective Polymerization of rac-Lactide
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC04834K
_journal_year                    2019
_chemical_formula_moiety         'C48 H60 N4 O Si2 Zn'
_chemical_formula_sum            'C48 H60 N4 O Si2 Zn'
_chemical_formula_weight         830.55
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2018-04-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.03 svn.r3497 for OlexSys, GUI svn.r5486)
;
_audit_update_record
;
2019-05-29 deposited with the CCDC.    2019-07-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.1380(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.78250(10)
_cell_length_b                   41.7789(6)
_cell_length_c                   11.4854(2)
_cell_measurement_reflns_used    9906
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      54.69
_cell_measurement_theta_min      4.107
_cell_volume                     4721.56(12)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      169.99
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_av_unetI/netI     0.0390
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -50
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            36826
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.899
_diffrn_reflns_theta_min         4.106
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.940
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.6258
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0992 before and 0.0574 after correction. The Ratio of minimum to maximum transmission is 0.8335. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.168
_exptl_crystal_description       block
_exptl_crystal_F_000             1768
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.690
_refine_diff_density_min         -0.735
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     567
_refine_ls_number_reflns         8922
_refine_ls_number_restraints     108
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0772
_refine_ls_R_factor_gt           0.0608
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0569P)^2^+8.1638P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1395
_refine_ls_wR_factor_ref         0.1519
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7163
_reflns_number_total             8922
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc04834k2.cif
_cod_data_source_block           mjl18142_0m
_cod_database_code               7123921
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.929
_shelx_estimated_absorpt_t_min   0.872
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C25 \\sim C30 \\sim C29 \\sim C28 \\sim C27 \\sim C26: within 2A with sigma of
0.005 and sigma for terminal atoms of 0.01
Uanis(C48) \\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C44)
\\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C46) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.01
Uanis(C16) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C27)
\\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C29) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.01
3. Others
 Fixed Sof: C17(0.5) H17(0.5) C18(0.5) H18A(0.5) H18B(0.5) C19(0.5) H19A(0.5)
 H19B(0.5) C20(0.5) H20A(0.5) H20B(0.5) C21(0.5) H21A(0.5) H21B(0.5) C22(0.5)
 H22A(0.5) H22B(0.5) C17'(0.5) H17'(0.5) C18'(0.5) H18C(0.5) H18D(0.5)
 C19'(0.5) H19C(0.5) H19D(0.5) C20'(0.5) H20C(0.5) H20D(0.5) C21'(0.5)
 H21C(0.5) H21D(0.5) C22'(0.5) H22C(0.5) H22D(0.5)
4.a Ternary CH refined with riding coordinates:
 C17(H17), C17'(H17')
4.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B),
 C21(H21A,H21B), C22(H22A,H22B), C18'(H18C,H18D), C19'(H19C,H19D), C20'(H20C,
 H20D), C21'(H21C,H21D), C22'(H22C,H22D)
4.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C11(H11), C12(H12), C13(H13), C14(H14), C26(H26), C27(H27),
 C28(H28), C29(H29), C30(H30), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36),
  C38(H38), C39(H39), C40(H40), C41(H41), C42(H42)
4.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C23(H23A,H23B,H23C), C43(H43A,H43B,H43C), C44(H44A,H44B,
 H44C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C48(H48A,
 H48B,H48C)
;
_shelx_res_checksum              97879
_shelx_fab_checksum              14977
_olex2_submission_special_instructions 'No special instructions were received'