Stereoselective polymerization of rac-lactide catalyzed by zwitterionic calcium complexes
Liu, Na; Liu, Doudou; Liu, Bo; Zhang, Hao; Cui, Dongmei; Polymer Chemistry 12 (2021) 1518–1525; doi:10.1039/D0PY01397H

data_1559799
_publ_section_title
;
 Stereoselective polymerization of rac-lactide catalyzed by zwitterionic
 calcium complexes
;
_journal_issue                   10
_journal_name_full               'Polymer Chemistry'
_journal_page_first              1518
_journal_page_last               1525
_journal_paper_doi               10.1039/D0PY01397H
_journal_volume                  12
_journal_year                    2021
_chemical_formula_moiety         'C36 H50 Ca N6 O P Si2'
_chemical_formula_sum            'C36 H50 Ca N6 O P Si2'
_chemical_formula_weight         710.05
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-09-29
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2020-12-14 deposited with the CCDC.	2020-12-15 downloaded from the CCDC.
;
_cell_angle_alpha                71.3370(10)
_cell_angle_beta                 73.9270(10)
_cell_angle_gamma                77.8820(10)
_cell_formula_units_Z            2
_cell_length_a                   9.9377(8)
_cell_length_b                   13.2229(10)
_cell_length_c                   17.1785(13)
_cell_measurement_reflns_used    3553
_cell_measurement_temperature    184.5
_cell_measurement_theta_max      23.683
_cell_measurement_theta_min      2.349
_cell_volume                     2036.7(3)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      184.5
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0160
_diffrn_reflns_av_unetI/netI     0.0370
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11696
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.397
_diffrn_reflns_theta_min         1.640
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.286
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.629929
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.0285 before and 0.0147 after correction.
The Ratio of minimum to maximum transmission is 0.6299.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.158
_exptl_crystal_description       block
_exptl_crystal_F_000             758
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.586
_refine_diff_density_min         -0.526
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     497
_refine_ls_number_reflns         8115
_refine_ls_number_restraints     107
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0852
_refine_ls_R_factor_gt           0.0601
_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^)+(0.0994P)^2^+0.4346P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1640
_refine_ls_wR_factor_ref         0.1875
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5583
_reflns_number_total             8115
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0py01397h2.cif
_cod_data_source_block           complex_2
_cod_depositor_comments
'Adding full bibliography for 1559799--1559800.cif.'
_cod_database_code               1559799
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.972
_shelx_estimated_absorpt_t_min   0.966
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C35-Si2
 2 with sigma of 0.02
 Si2-C36 \\sim Si2-C35 \\sim Si2-C32
 with sigma of 0.02
 Si2'-C37 \\sim Si2'-C39 \\sim Si2'-C38
 with sigma of 0.02
 Si2-N6 \\sim Si2'-N6
 with sigma of 0.02
 Si1-C34 \\sim Si1-C28 \\sim Si1-C33B
 with sigma of 0.02
 Si1-C34 \\sim Si1-C40
 with sigma of 0.02
 Si1-C33A \\sim Si1-C33B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C34 \\sim C40: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
C33A \\sim C33B: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
Uanis(C33A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 Si2', C38, C39, C37, N6
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Si2, C35, C36, C32, N6
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C33B, Si1, C28, C34
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C33A, Si1, C33B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(Si2')=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(H37C)=Sof(C38)=Sof(H38A)=Sof(H38B)=
 Sof(H38C)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=1-FVAR(1)
 Sof(Si2)=Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=Sof(C35)=Sof(H35A)=Sof(H35B)=
 Sof(H35C)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=FVAR(1)
 Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=1-FVAR(2)
 Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(H40C)=FVAR(2)
 Sof(C33B)=Sof(H33A)=Sof(H33B)=Sof(H33C)=1-FVAR(3)
 Sof(C33A)=Sof(H33D)=Sof(H33E)=Sof(H33F)=FVAR(3)
6.a Ternary CH refined with riding coordinates:
 C7(H7)
6.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C13(H13),
 C17(H17), C18(H18), C19(H19), C22(H22), C23(H23), C24(H24), C26(H26), C30(H30)
6.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C28(H28A,H28B,
 H28C), C29(H29A,H29B,H29C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C),
 C33B(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,
 H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,
 H40B,H40C), C33A(H33D,H33E,H33F)
;
_shelx_res_checksum              2722
_olex2_submission_special_instructions 'No special instructions were received'