Stereoselective Alkali-Metal Catalysts for Highly Isotactic Poly(rac-lactide) Synthesis.
Sun, Yangyang; Xiong, Jiao; Dai, Zhongran; Pan, Xiaobo; Tang, Ning; Wu, Jincai; Inorganic chemistry 55 (2015) 136–; doi:10.1021/acs.inorgchem.5b02709

data_4344768
_publ_section_title
;
 Stereoselective Alkali-Metal Catalysts for Highly Isotactic
 Poly(rac-lactide) Synthesis.
;
_journal_issue                   1
_journal_name_full               'Inorganic chemistry'
_journal_page_first              136
_journal_paper_doi               10.1021/acs.inorgchem.5b02709
_journal_volume                  55
_journal_year                    2015
_chemical_formula_moiety         'C40 H53 K O7'
_chemical_formula_sum            'C40 H53 K O7'
_chemical_formula_weight         684.92
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-06-04
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 103.147(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.2808(13)
_cell_length_b                   22.016(2)
_cell_length_c                   19.332(3)
_cell_measurement_reflns_used    2468
_cell_measurement_temperature    290.92(10)
_cell_measurement_theta_max      24.7000
_cell_measurement_theta_min      3.7230
_cell_volume                     3846.5(9)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      290.92(10)
_diffrn_detector_area_resol_mean 16.0733
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.818
_diffrn_measurement_details
;
  1 omega  -15.00   11.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.3571  -99.0000  120.0000 26

  2 omega  -13.00   26.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.3571  -99.0000  -60.0000 39

  3 omega  -49.00   19.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7946  -57.0000  120.0000 68

  4 omega   -2.00   89.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7946   57.0000  -90.0000 91

  5 omega   40.00   72.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7946  178.0000   90.0000 32
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0619964000
_diffrn_orient_matrix_UB_12      -0.0161499000
_diffrn_orient_matrix_UB_13      -0.0198312000
_diffrn_orient_matrix_UB_21      0.0316039000
_diffrn_orient_matrix_UB_22      0.0005422000
_diffrn_orient_matrix_UB_23      -0.0301094000
_diffrn_orient_matrix_UB_31      0.0364416000
_diffrn_orient_matrix_UB_32      -0.0278655000
_diffrn_orient_matrix_UB_33      0.0108856000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0656
_diffrn_reflns_av_unetI/netI     0.0978
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            19025
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.14
_diffrn_reflns_theta_min         3.38
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.184
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91203
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.495
_refine_diff_density_min         -0.458
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         8488
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1460
_refine_ls_R_factor_gt           0.0833
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0940P)^2^+1.6210P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1942
_refine_ls_wR_factor_ref         0.2463
_reflns_number_gt                4678
_reflns_number_total             8488
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b02709_si_005.cif
_cod_data_source_block           sunyy1211
_cod_original_cell_volume        3846.6(8)
_cod_database_code               4344768
_reflns_odcompleteness_completeness 94.64
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.a Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C38(H38A,H38B), C39(H39A,H39B), C32(H32A,H32B), C37(H37A,
 H37B), C36(H36A,H36B), C31(H31A,H31B), C34(H34A,H34B), C35(H35A,H35B),
 C29(H29A,H29B), C40(H40A,H40B), C30(H30A,H30B)
2.b Me refined as rotating group:
 C23(H23A,H23B,H23C)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C19(H19), C14(H14), C18(H18), C17(H17), C9(H9), C5(H5), C16(H16),
 C10(H10), C11(H11), C12(H12)
2.d Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C27(H27A,H27B,H27C), C26(H26A,H26B,H26C), C22(H22A,H22B,
 H22C), C28(H28A,H28B,H28C)
;
_olex2_submission_special_instructions 'No special instructions were received'