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_4344766
_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         'C32 H37 K O7, C3 H3'
_chemical_formula_sum            'C35 H40 K O7'
_chemical_formula_weight         611.77
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-05-20
_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                 91.238(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.5706(10)
_cell_length_b                   10.8792(5)
_cell_length_c                   28.0601(16)
_cell_measurement_reflns_used    1876
_cell_measurement_temperature    173.73
_cell_measurement_theta_max      25.1730
_cell_measurement_theta_min      3.8120
_cell_volume                     6278.2(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      173.73
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0733
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega   -5.00   93.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854   38.0000  120.0000 98

  2 omega   35.00   75.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854  178.0000  120.0000 40

  3 omega   35.00   97.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854  178.0000  -30.0000 62

  4 omega  -47.00   -6.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854  -57.0000  150.0000 41
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0050224000
_diffrn_orient_matrix_UB_12      -0.0036005000
_diffrn_orient_matrix_UB_13      -0.0249145000
_diffrn_orient_matrix_UB_21      -0.0211990000
_diffrn_orient_matrix_UB_22      -0.0512410000
_diffrn_orient_matrix_UB_23      -0.0015757000
_diffrn_orient_matrix_UB_31      -0.0267252000
_diffrn_orient_matrix_UB_32      0.0400573000
_diffrn_orient_matrix_UB_33      -0.0041953000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0558
_diffrn_reflns_av_unetI/netI     0.0933
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            13247
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         3.48
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.217
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98614
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2600
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.284
_refine_diff_density_min         -0.305
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     396
_refine_ls_number_reflns         6188
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0983
_refine_ls_R_factor_gt           0.0563
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0228P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0906
_refine_ls_wR_factor_ref         0.1091
_reflns_number_gt                3998
_reflns_number_total             6188
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b02709_si_002.cif
_cod_data_source_block           sunyy0105
_cod_original_cell_volume        6278.1(6)
_cod_database_code               4344766
_reflns_odcompleteness_completeness 99.72
_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
2. Restrained distances
 H22B-C22
 0.97 with sigma of 0.02
 C22-H22A
 0.97 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,
 H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B),
 C31(H31A,H31B), C32(H32A,H32B)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C19(H19), C18(H18), C17(H17), C16(H16),
 C14(H14), C12(H12), C11(H11), C10(H10), C9(H9), C34(H34), C33(H33), C35(H35)
;
_olex2_date_sample_data_collection 2015-01-05
_olex2_submission_special_instructions 'No special instructions were received'