Controlled Synthesis of Polycarbonate Diols and Their Polylactide Block Copolymers using Amino-bis(phenolate) Chromium Hydroxide Complexes
Ni, Kaijie; Dawe, Louise N.; Sarjeant, Amy; Kozak, Christopher M.; Dalton Transactions  (2023) –; doi:10.1039/D3DT03168C

data_7714402
_publ_section_title
;
 Controlled Synthesis of Polycarbonate Diols and Their Polylactide Block
 Copolymers using Amino-bis(phenolate) Chromium Hydroxide Complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT03168C
_journal_year                    2023
_chemical_formula_moiety         'C66 H104 Cr2 N2 O8'
_chemical_formula_sum            'C66 H104 Cr2 N2 O8'
_chemical_formula_weight         1157.51
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-11-02
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-11-02 deposited with the CCDC.	2023-11-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.150(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.509(5)
_cell_length_b                   17.346(5)
_cell_length_c                   29.415(8)
_cell_measurement_reflns_used    3292
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      23.853
_cell_measurement_theta_min      2.195
_cell_volume                     8699(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2008)'
_diffrn_ambient_temperature      153.15
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0452
_diffrn_reflns_av_unetI/netI     0.1009
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            29311
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         2.611
_exptl_absorpt_coefficient_mu    0.289
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4762
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/2 (Bruker,2014/2) was used for absorption correction.
wR2(int) was 0.0662 before and 0.0454 after correction.
The Ratio of minimum to maximum transmission is 0.6389.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'Dark Green'
_exptl_crystal_density_diffrn    0.884
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2504
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.549
_refine_diff_density_min         -0.801
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.160
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     720
_refine_ls_number_reflns         15222
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      1.160
_refine_ls_R_factor_all          0.1686
_refine_ls_R_factor_gt           0.1105
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3459
_refine_ls_wR_factor_ref         0.3753
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7687
_reflns_number_total             15222
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03168c2.cif
_cod_data_source_block           jb008
_cod_database_code               7714402
_shelx_shelxl_version_number     2018/3
_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, All O(H) groups
2. Restrained distances
 O7-H7
 0.85 with sigma of 0.02
 O8-H8
 0.85 with sigma of 0.02
 C25A-C22 \\sim C25-C22 \\sim C24A-C22 \\sim C24-C22 \\sim C23A-C22 \\sim
C23-C22
 with sigma of 0.02
 C25-C24 \\sim C24-C23
 with sigma of 0.02
 C25A-C24A \\sim C24A-C23A
 with sigma of 0.02
 C56A-C55A \\sim C58A-C55A \\sim C57A-C55A
 with sigma of 0.02
 C56A-C58A \\sim C58A-C57A
 with sigma of 0.02
 C57-C55 \\sim C58-C55 \\sim C56-C55
 with sigma of 0.02
 C57-C58 \\sim C58-C56
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C55A) = Uanis(C55) = Uanis(C56) = Uanis(C58A) = Uanis(C58) = Uanis(C56A)
= Uanis(C57) = Uanis(C57A)
Uanis(C24A) = Uanis(C23)
Uanis(C24) = Uanis(C25A)
4. Rigid body (RIGU) restrains
 C22, C23, C23A, C24, C24A, C25, C25A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Sof(C23A)=Sof(H23D)=Sof(H23E)=Sof(H23F)=Sof(C24A)=Sof(H24D)=Sof(H24E)=
 Sof(H24F)=Sof(C25A)=Sof(H25D)=Sof(H25E)=Sof(H25F)=1-FVAR(1)
 Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=
 Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=FVAR(1)
 Sof(C55)=Sof(C56)=Sof(H56A)=Sof(H56B)=Sof(H56C)=Sof(C57)=Sof(H57A)=Sof(H57B)=
 Sof(H57C)=Sof(C58)=Sof(H58A)=Sof(H58B)=Sof(H58C)=1-FVAR(2)
 Sof(C55A)=Sof(C56A)=Sof(H56D)=Sof(H56E)=Sof(H56F)=Sof(C57A)=Sof(H57D)=
 Sof(H57E)=Sof(H57F)=Sof(C58A)=Sof(H58D)=Sof(H58E)=Sof(H58F)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C15(H15A,H15B), C16(H16A,H16B), C40(H40A,H40B),
 C41(H41A,H41B), C48(H48A,H48B), C49(H49A,H49B)
6.b Me refined with riding coordinates:
 C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C23(H23A,H23B,H23C), C23A(H23D,H23E,H23F), C24(H24A,H24B,H24C),
 C24A(H24D,H24E,H24F), C25(H25A,H25B,H25C), C25A(H25D,H25E,H25F), C27(H27A,H27B,
 H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C31(H31A,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), C56(H56A,H56B,H56C), C56A(H56D,H56E,
 H56F), C57(H57A,H57B,H57C), C57A(H57D,H57E,H57F), C58(H58A,H58B,H58C),
 C58A(H58D,H58E,H58F), C60(H60A,H60B,H60C), C61(H61A,H61B,H61C), C62(H62A,H62B,
 H62C), C64(H64A,H64B,H64C), C65(H65A,H65B,H65C), C66(H66A,H66B,H66C)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C10(H10), C12(H12), C36(H36), C38(H38), C43(H43), C45(H45)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              96534
_shelx_fab_checksum              16638
_olex2_submission_special_instructions 'No special instructions were received'