Bimetallic and trimetallic zinc amino-bis(phenolate) complexes for ring-opening polymerization of rac-lactide.
Liu, Yi; Dawe, Louise N.; Kozak, Christopher M.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 13699–13710; doi:10.1039/c9dt03118a

data_7700954
_publ_section_title
;
 Bimetallic and trimetallic zinc amino-bis(phenolate) complexes for
 ring-opening polymerization of rac-lactide.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13699
_journal_page_last               13710
_journal_paper_doi               10.1039/c9dt03118a
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C72 H116 N2 O6 Zn3'
_chemical_formula_sum            'C72 H116 N2 O6 Zn3'
_chemical_formula_weight         1301.77
_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
_audit_creation_date             2014-11-01
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_audit_update_record
;
2015-07-11 deposited with the CCDC.    2019-08-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.2080(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.4644(9)
_cell_length_b                   28.1652(19)
_cell_length_c                   20.0841(14)
_cell_measurement_reflns_used    9860
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      27.99
_cell_measurement_theta_min      2.20
_cell_volume                     7383.5(9)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2008)'
_diffrn_ambient_temperature      125.02
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.966
_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  0.0533
_diffrn_reflns_av_unetI/netI     0.0621
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            60031
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.292
_diffrn_reflns_theta_min         2.092
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.014
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6838
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0755 before and 0.0482 after correction.
The Ratio of minimum to maximum transmission is 0.9170.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.171
_exptl_crystal_description       amorphous
_exptl_crystal_F_000             2800
_exptl_crystal_size_max          0.354
_exptl_crystal_size_mid          0.251
_exptl_crystal_size_min          0.226
_refine_diff_density_max         0.414
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     840
_refine_ls_number_reflns         17705
_refine_ls_number_restraints     102
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0805
_refine_ls_R_factor_gt           0.0426
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0427P)^2^+0.4332P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0871
_refine_ls_wR_factor_ref         0.0995
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11774
_reflns_number_total             17705
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03118a2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7700953--7700954.cif.'
_cod_database_code               7700954
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.803
_shelx_estimated_absorpt_t_min   0.715
_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
 C57A-C55 \\sim C56-C55 \\sim C56A-C55 \\sim C58-C55 \\sim C58A-C55 \\sim
C57-C55
 with sigma of 0.02
 C62A-C59 \\sim C60-C59 \\sim C60A-C59 \\sim C61-C59 \\sim C61c-C59 \\sim
C62-C59
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C55, C57A, C56, C56A, C58, C58A, C57
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C59, C62, C62A, C60, C60A, C61, C61c
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C56A)=Sof(H56A)=Sof(H56B)=Sof(H56C)=Sof(C57A)=Sof(H57A)=Sof(H57B)=
 Sof(H57C)=Sof(C58A)=Sof(H58A)=Sof(H58B)=Sof(H58C)=1-FVAR(1)
 Sof(C56)=Sof(H56D)=Sof(H56E)=Sof(H56F)=Sof(C57)=Sof(H57D)=Sof(H57E)=Sof(H57F)=
 Sof(C58)=Sof(H58D)=Sof(H58E)=Sof(H58F)=FVAR(1)
 Sof(C60A)=Sof(H60D)=Sof(H60E)=Sof(H60F)=Sof(C61c)=Sof(H61c)=Sof(H61B)=
 Sof(H61C)=Sof(C62A)=Sof(H62D)=Sof(H62E)=Sof(H62F)=1-FVAR(2)
 Sof(C60)=Sof(H60A)=Sof(H60B)=Sof(H60C)=Sof(C61)=Sof(H61D)=Sof(H61E)=Sof(H61F)=
 Sof(C62)=Sof(H62A)=Sof(H62B)=Sof(H62C)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C67(H67), C70(H70)
5.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C15(H15A,H15B), C16(H16A,H16B), C40(H40A,H40B),
 C41(H41c,H41B), C48(H48A,H48B), C49(H49A,H49B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C10(H10), C12(H12), C36(H36), C38(H38), C43(H43), C45(H45)
5.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21c,H21B,
 H21C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C27(H27A,
 H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C31(H31c,H31B,H31C),
 C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C50(H50A,H50B,H50C), C52(H52A,H52B,
 H52C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C56A(H56A,H56B,H56C),
 C56(H56D,H56E,H56F), C57A(H57A,H57B,H57C), C57(H57D,H57E,H57F), C58A(H58A,H58B,
 H58C), C58(H58D,H58E,H58F), C60(H60A,H60B,H60C), C60A(H60D,H60E,H60F),
 C61c(H61c,H61B,H61C), C61(H61D,H61E,H61F), C62(H62A,H62B,H62C), C62A(H62D,H62E,
 H62F), C64(H64A,H64B,H64C), C65(H65A,H65B,H65C), C66(H66A,H66B,H66C), C68(H68A,
 H68B,H68C), C69(H69A,H69B,H69C), C71(H71c,H71B,H71C), C72(H72A,H72B,H72C)
;
_shelx_res_checksum              68203
_olex2_submission_special_instructions 'No special instructions were received'