Potassium complexes supported by monoanionic tetradentate amino-phenolate ligands: synthesis, structure and catalysis in ring-opening polymerization of rac-lactide
Yao, Chenhui; Yang, Yang; Xu, Shaoan; ma, haiyan; Dalton Trans.  (2017) –; doi:10.1039/C7DT00812K

data_7042638
_publ_section_title
;
 Potassium complexes supported by monoanionic tetradentate amino-phenolate
 ligands: synthesis, structure and catalysis in ring-opening
 polymerization of rac-lactide
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT00812K
_journal_year                    2017
_chemical_formula_moiety         'C80 H106 K2 N6 O2'
_chemical_formula_sum            'C80 H106 K2 N6 O2'
_chemical_formula_weight         1261.90
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-01-12
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_audit_update_record
;
2017-03-03 deposited with the CCDC.
2017-04-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.3480(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.1335(15)
_cell_length_b                   13.8361(9)
_cell_length_c                   24.8293(17)
_cell_measurement_reflns_used    9990
_cell_measurement_temperature    130
_cell_measurement_theta_max      27.396
_cell_measurement_theta_min      2.22
_cell_volume                     7818.0(9)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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      130
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_av_unetI/netI     0.0534
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            79715
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.499
_diffrn_reflns_theta_max         30.55
_diffrn_reflns_theta_min         0.83
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.167
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.7074
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0490 before and 0.0424 after correction.
The Ratio of minimum to maximum transmission is 0.9481.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.072
_exptl_crystal_description       block
_exptl_crystal_F_000             2728
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.670
_refine_diff_density_min         -0.851
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     835
_refine_ls_number_reflns         14479
_refine_ls_number_restraints     129
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0973
_refine_ls_R_factor_gt           0.0734
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1249P)^2^+12.5605P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1969
_refine_ls_wR_factor_ref         0.2270
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10722
_reflns_number_total             14479
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00812k2.cif
_cod_data_source_block           mo_dm16262_0m
_cod_database_code               7042638
_shelx_estimated_absorpt_t_max   0.959
_shelx_estimated_absorpt_t_min   0.948
_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. Restrained distances
 C80-C79
 1.52 with sigma of 0.02
3. Rigid bond restraints
 N4, C79
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C79, C80
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
N4 \\sim C77 \\sim C78 \\sim C79 \\sim C80: within 2A with sigma of 0.005 and
sigma for terminal atoms of 0.01
C17 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25: within 2A with
sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C80) \\sim Ueq, Uanis(C79) \\sim Ueq, Uanis(C77) \\sim Ueq, Uanis(C78)
\\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C22) \\sim Ueq,
Uanis(C23) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C25) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C21(H21A,H21B), C22(H22A,H22B), C26(H26A,H26B), C35(H35A,H35B),
 C36(H36A,H36B), C37(H37A,H37B), C39(H39A,H39B), C41(H41A,H41B), C66(H66A,H66B),
  C76(H76A,H76B), C77(H77A,H77B), C79(H79A,H79B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C23(H23),
 C24(H24), C25(H25), C28(H28), C29(H29), C30(H30), C31(H31), C43(H43), C45(H45),
  C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C61(H61), C62(H62),
 C63(H63), C64(H64), C65(H65), C69(H69), C70(H70), C71(H71), C72(H72)
5.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C18(H18A,H18B,H18C), C19(H19A,H19B,
 H19C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C38(H38A,H38B,H38C), C40(H40A,
 H40B,H40C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C58(H58A,H58B,H58C),
 C59(H59A,H59B,H59C), C73(H73A,H73B,H73C), C74(H74A,H74B,H74C), C78(H78A,H78B,
 H78C), C80(H80A,H80B,H80C)
;
_shelx_res_checksum              73068
_shelx_fab_checksum              26394
_shelx_shelxl_version_number     2016/6
_olex2_submission_special_instructions 'No special instructions were received'