Why So Slow? Mechanistic Insights from Studies of a Poor Catalyst for Polymerization of ε-Caprolactone.
Stasiw, Daniel E.; Mandal, Mukunda; Neisen, Benjamin D.; Mitchell, Lauren A.; Cramer, Christopher J.; Tolman, William B.; Inorganic chemistry 56 (2017) 725–728; doi:10.1021/acs.inorgchem.6b02849

data_4345093
_publ_section_title
;
 Why So Slow? Mechanistic Insights from Studies of a Poor Catalyst for
 Polymerization of \e-Caprolactone.
;
_journal_issue                   2
_journal_name_full               'Inorganic chemistry'
_journal_page_first              725
_journal_page_last               728
_journal_paper_doi               10.1021/acs.inorgchem.6b02849
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety         '2(C24 H27 Al N4 O), C4 H10 O'
_chemical_formula_sum            'C52 H64 Al2 N8 O3'
_chemical_formula_weight         903.07
_chemical_name_systematic        AlOEtTMTAA
_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   geom
_audit_creation_date             2016-09-29
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_cell_angle_alpha                90
_cell_angle_beta                 104.0000(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.2027(3)
_cell_length_b                   9.8304(3)
_cell_length_c                   18.8076(5)
_cell_measurement_reflns_used    9951
_cell_measurement_temperature    123.0
_cell_measurement_theta_max      74.50
_cell_measurement_theta_min      3.71
_cell_volume                     2368.49(11)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'APEX II, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_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      123
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0475
_diffrn_reflns_av_unetI/netI     0.0152
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            56485
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.500
_diffrn_reflns_theta_min         3.705
_exptl_absorpt_coefficient_mu    0.967
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_density_meas      ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             964
_exptl_crystal_recrystallization_method
'crystallized by slow diffusion of pentane into diethyl ether'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   0.908
_exptl_transmission_factor_min   0.890
_refine_diff_density_max         0.233
_refine_diff_density_min         -0.235
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     324
_refine_ls_number_reflns         4835
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0333
_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^)+(0.0498P)^2^+0.8029P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0850
_refine_ls_wR_factor_ref         0.0881
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4448
_reflns_number_total             4835
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02849_si_002.cif
_cod_data_source_block           shelx
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 
;
_cod_database_code               4345093
_shelxl_version_number           2014/6
_olex2_refinement_description
;
1. Others
 Fixed Sof: C25(0.5) H25A(0.5) H25B(0.5) H25C(0.5) C26(0.5) H26A(0.5)
 H26B(0.5) O2(0.5) C27(0.5) H27A(0.5) H27B(0.5) C28(0.5) H28A(0.5) H28B(0.5)
 H28C(0.5)
 Fixed Uiso: H1A(0.038) H1B(0.038) H1C(0.038) H3(0.025) H5A(0.038) H5B(0.038)
 H5C(0.038) H7(0.031) H8(0.036) H9(0.035) H10(0.029) H12A(0.037) H12B(0.037)
 H12C(0.037) H14(0.023) H16A(0.035) H16B(0.035) H16C(0.035) H18(0.026)
 H19(0.03) H20(0.031) H21(0.028) H23A(0.035) H23B(0.035) H24A(0.093)
 H24B(0.093) H24C(0.093) H25A(0.153) H25B(0.153) H25C(0.153) H26A(0.111)
 H26B(0.111) H27A(0.094) H27B(0.094) H28A(0.142) H28B(0.142) H28C(0.142)
 Fixed X: H1A(0.7335) H1B(0.7067) H1C(0.6463) H3(0.4814) H5A(0.248)
 H5B(0.3049) H5C(0.2846) H7(0.2426) H8(0.1154) H9(0.125) H10(0.2625)
 H12A(0.2756) H12B(0.3215) H12C(0.3454) H14(0.5223) H16A(0.6857) H16B(0.7462)
 H16C(0.7615) H18(0.8322) H19(0.9788) H20(0.968) H21(0.8107) H23A(0.4987)
 H23B(0.5882) H24A(0.4774) H24B(0.3879) H24C(0.4285) H25A(0.0657) H25B(0.0211)
 H25C(0.1215) H26A(-0.0796) H26B(-0.0156) H27A(-0.0304) H27B(-0.0935)
 H28A(0.1026) H28B(-0.0025) H28C(0.0352)
 Fixed Y: H1A(0.9392) H1B(1.0389) H1C(1.0494) H3(1.0177) H5A(0.867)
 H5B(0.9959) H5C(0.9825) H7(0.8048) H8(0.6585) H9(0.4283) H10(0.3413)
 H12A(0.3687) H12B(0.2337) H12C(0.2746) H14(0.2784) H16A(0.3202) H16B(0.2813)
 H16C(0.4254) H18(0.4118) H19(0.5334) H20(0.765) H21(0.8783) H23A(0.7254)
 H23B(0.6481) H24A(0.4612) H24B(0.5396) H24C(0.5916) H25A(0.2377) H25B(0.1277)
 H25C(0.2101) H26A(0.3165) H26B(0.3001) H27A(0.542) H27B(0.5567) H28A(0.6759)
 H28B(0.7574) H28C(0.6952)
 Fixed Z: H1A(0.5976) H1B(0.6555) H1C(0.5729) H3(0.5828) H5A(0.5696)
 H5B(0.5491) H5C(0.6276) H7(0.6932) H8(0.7144) H9(0.6922) H10(0.6495)
 H12A(0.5221) H12B(0.5613) H12C(0.4865) H14(0.5228) H16A(0.5063) H16B(0.5861)
 H16C(0.5546) H18(0.6845) H19(0.7443) H20(0.7625) H21(0.7217) H23A(0.8016)
 H23B(0.8568) H24A(0.8538) H24B(0.7993) H24C(0.88) H25A(0.4242) H25B(0.4688)
 H25C(0.5065) H26A(0.4622) H26B(0.5439) H27A(0.5614) H27B(0.4791) H28A(0.5351)
 H28B(0.5208) H28C(0.4548)
;
_shelx_res_checksum              93801
_shelx_hkl_checksum              94892
_olex2_submission_original_sample_id 16003_final
_olex2_submission_special_instructions 'No special instructions were received'