Configurationally flexible zinc complexes as catalysts for rac-lactide polymerisation.
Daneshmand, Pargol; Michalsky, Ina; Aguiar, Pedro M.; Schaper, Frank; Dalton transactions (Cambridge, England : 2003) 47 (2018) 16279–16291; doi:10.1039/c8dt02562b

data_7047808
_publ_section_title
;
 Configurationally flexible zinc complexes as catalysts for rac-lactide
 polymerisation.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16279
_journal_page_last               16291
_journal_paper_doi               10.1039/c8dt02562b
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C25 H47 N3 O Zn'
_chemical_formula_sum            'C25 H47 N3 O Zn'
_chemical_formula_weight         471.02
_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     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-11-27
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-06-19 deposited with the CCDC.
2018-10-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.843(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.9872(6)
_cell_length_b                   24.3367(16)
_cell_length_c                   11.7387(7)
_cell_measurement_reflns_used    9837
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      71.38
_cell_measurement_theta_min      5.30
_cell_volume                     2781.8(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection
'APEX 2 (2013) Bruker AXS Inc., Madison, WI 53719-1173.'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            31767
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.276
_diffrn_reflns_theta_min         5.306
_diffrn_source                   'Microfocus Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.350
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.6732
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/2 (Bruker,2014/2) was used for absorption correction. wR2(int) was 0.1262 before and 0.0413 after correction. The Ratio of minimum to maximum transmission is 0.8888. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.125
_exptl_crystal_description       block
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.709
_refine_diff_density_min         -1.162
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.271
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         5351
_refine_ls_number_restraints     272
_refine_ls_restrained_S_all      1.275
_refine_ls_R_factor_all          0.0882
_refine_ls_R_factor_gt           0.0586
_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^)+(0.1793P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1964
_refine_ls_wR_factor_ref         0.2791
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4211
_reflns_number_total             5351
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02562b2.cif
_cod_data_source_block           comp8
_cod_depositor_comments
'Adding full bibliography for 7047804--7047808.cif.'
_cod_database_code               7047808
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.923
_shelx_estimated_absorpt_t_min   0.813
_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
 C18A-N2A \\sim C18B-N2B \\sim C19A-N2A \\sim C19B-N2B
 with sigma of 0.001
 C18A-C19A \\sim C18B-C19B
 with sigma of 0.02
 C17A-N2A \\sim C17B-N2B
 with sigma of 0.001
 C16A-C17A \\sim C16B-C17B
 with sigma of 0.001
 N1-C16A \\sim N1-C16B
 with sigma of 0.001
 N1-C17A \\sim N1-C17B
 with sigma of 0.02
 N2A-C16A \\sim N2B-C16B
 with sigma of 0.02
 C8A-C9A \\sim C8A-C10A \\sim C8A-C11A \\sim C8B-C9B \\sim C8B-C10B \\sim
C8B-C11B
 with sigma of 0.001
 C9A-C10A \\sim C10A-C11A \\sim C11A-C9A \\sim C9B-C10B \\sim C10B-C11B \\sim
C11B-C9B
 with sigma of 0.02
 C4-C8A \\sim C4-C8B
 with sigma of 0.001
 C12A-C13A \\sim C12A-C14A \\sim C12A-C15A \\sim C12B-C13B \\sim C12B-C14B
\\sim C12B-C15B
 with sigma of 0.001
 C13A-C14A \\sim C14A-C15A \\sim C15A-C13A \\sim C13B-C14B \\sim C14B-C15B
\\sim C15B-C13B
 with sigma of 0.02
 C6-C12A \\sim C6-C12B
 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 0.8A with sigma of 0.002 and
sigma for terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 C16A, C17A, C18A, C19A, C16B, C17B, C18B, C19B, N2A, N2B, N1
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C8A, C9A, C10A, C11A, C8B, C9B, C10B, C11B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C12A, C13A, C14A, C15A, C12B, C13B, C14B, C15B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Sof(N2B)=Sof(C19B)=Sof(H19D)=Sof(H19E)=Sof(H19F)=Sof(C18B)=Sof(H18D)=
 Sof(H18E)=Sof(H18F)=Sof(C17B)=Sof(H17C)=Sof(H17D)=Sof(C16B)=Sof(H16C)=
 Sof(H16D)=1-FVAR(1)
 Sof(C16A)=Sof(H16A)=Sof(H16B)=Sof(C17A)=Sof(H17A)=Sof(H17B)=Sof(N2A)=
 Sof(C18A)=Sof(H18A)=Sof(H18B)=Sof(H18C)=Sof(C19A)=Sof(H19A)=Sof(H19B)=
 Sof(H19C)=FVAR(1)
 Sof(C11B)=Sof(H11D)=Sof(H11E)=Sof(H11F)=Sof(C10B)=Sof(H10D)=Sof(H10E)=
 Sof(H10F)=Sof(C9B)=Sof(H9BA)=Sof(H9BB)=Sof(H9BC)=Sof(C8B)=1-FVAR(2)
 Sof(C8A)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=Sof(C10A)=Sof(H10A)=Sof(H10B)=
 Sof(H10C)=Sof(C11A)=Sof(H11A)=Sof(H11B)=Sof(H11C)=FVAR(2)
 Sof(C15B)=Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(C12B)=Sof(C13B)=Sof(H13D)=
 Sof(H13E)=Sof(H13F)=Sof(C14B)=Sof(H14D)=Sof(H14E)=Sof(H14F)=1-FVAR(3)
 Sof(C12A)=Sof(C13A)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C14A)=Sof(H14A)=
 Sof(H14B)=Sof(H14C)=Sof(C15A)=Sof(H15A)=Sof(H15B)=Sof(H15C)=FVAR(3)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C20(H20A,H20B), C21(H21A,H21B), C24(H24A,H24B), C16A(H16A,H16B),
 C17A(H17A,H17B), C17B(H17C,H17D), C16B(H16C,H16D)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5)
6.c Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C18A(H18A,H18B,
 H18C), C19A(H19A,H19B,H19C), C19B(H19D,H19E,H19F), C18B(H18D,H18E,H18F),
 C9A(H9AA,H9AB,H9AC), C10A(H10A,H10B,H10C), C11A(H11A,H11B,H11C), C11B(H11D,
 H11E,H11F), C10B(H10D,H10E,H10F), C9B(H9BA,H9BB,H9BC), C13A(H13A,H13B,H13C),
 C14A(H14A,H14B,H14C), C15A(H15A,H15B,H15C), C15B(H15D,H15E,H15F), C13B(H13D,
 H13E,H13F), C14B(H14D,H14E,H14F)
;
_shelx_res_checksum              57327
_olex2_submission_special_instructions 'No special instructions were received'