Dinuclear iminophenoxide copper complexes in rac-lactide polymerisation.
Daneshmand, Pargol; Pinon, Leena; Schaper, Frank; Dalton transactions (Cambridge, England : 2003) 47 (2018) 10147–10161; doi:10.1039/c8dt02140f

data_7046974
_publ_section_title
;
 Dinuclear iminophenoxide copper complexes in rac-lactide polymerisation.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10147
_journal_page_last               10161
_journal_paper_doi               10.1039/c8dt02140f
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C64 H84 Cu2 N4 O4'
_chemical_formula_sum            'C64 H84 Cu2 N4 O4'
_chemical_formula_weight         1100.43
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-12-05
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-05-24 deposited with the CCDC.
2018-07-05 downloaded from the CCDC.
;
_cell_angle_alpha                82.603(2)
_cell_angle_beta                 88.935(2)
_cell_angle_gamma                74.196(2)
_cell_formula_units_Z            1
_cell_length_a                   10.9595(5)
_cell_length_b                   11.4816(5)
_cell_length_c                   12.5663(5)
_cell_measurement_reflns_used    9963
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      60.69
_cell_measurement_theta_min      3.09
_cell_volume                     1508.59(11)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_detector_area_resol_mean 10.24
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker Venture Metaljet'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0593
_diffrn_reflns_av_unetI/netI     0.0358
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            43024
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         60.782
_diffrn_reflns_theta_min         3.086
_diffrn_source                   'Metal Jet'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.049
_exptl_absorpt_correction_T_max  0.7519
_exptl_absorpt_correction_T_min  0.5791
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/2 (Bruker,2014/2) was used for absorption correction. wR2(int) was 0.1002 before and 0.0729 after correction. The Ratio of minimum to maximum transmission is 0.7702. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.211
_exptl_crystal_description       block
_exptl_crystal_F_000             586
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.577
_refine_diff_density_min         -0.501
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         6935
_refine_ls_number_restraints     242
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0721
_refine_ls_R_factor_gt           0.0627
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1040P)^2^+1.1211P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1606
_refine_ls_wR_factor_ref         0.1689
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6091
_reflns_number_total             6935
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02140f2.cif
_cod_data_source_block           comp_10a
_cod_depositor_comments
'Adding full bibliography for 7046963--7046983.cif.'
_cod_database_code               7046974
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.642
_shelx_estimated_absorpt_t_min   0.564
_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
 H24B_$1-H11B
 -2.41 with sigma of 0.02
 C23A-C24A \\sim C24A-C25A \\sim C25A-C26A \\sim C26A-C27A \\sim C27A-C28A
\\sim C28A-C23A \\sim C23B-
 C24B \\sim C24B-C25B \\sim C25B-C26B \\sim C26B-C27B \\sim C27B-C28B \\sim
C28B-C23B
 with sigma of 0.001
 C23A-C25A \\sim C24A-C26A \\sim C25A-C27A \\sim C26A-C28A \\sim C27A-C23A
\\sim C28A-C24A \\sim C23B-
 C25B \\sim C24B-C26B \\sim C25B-C27B \\sim C26B-C28B \\sim C27B-C23B \\sim
C28B-C24B
 with sigma of 0.02
 C16-C23A \\sim C16-C23B
 with sigma of 0.001
 C16-C28A \\sim C16-C28B \\sim C16-C24A \\sim C16-C24B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 0.8A with sigma of 0.02 and sigma
for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C23A, C24A, C25A, C26A, C27A, C28A, C23B, C24B, C25B, C26B, C27B, C28B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H16)=Sof(C23A)=Sof(C28A)=Sof(H28A)=Sof(C27A)=Sof(H27A)=Sof(C26A)=
 Sof(H26A)=Sof(C25A)=Sof(H25A)=Sof(C24A)=Sof(H24A)=1-FVAR(1)
 Sof(H16A)=Sof(C23B)=Sof(C24B)=Sof(H24B)=Sof(C25B)=Sof(H25B)=Sof(C26B)=
 Sof(H26B)=Sof(C27B)=Sof(H27B)=Sof(C28B)=Sof(H28B)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C16(H16A), C16(H16)
6.b Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C30(H30A,H30B)
6.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C5(H5), C7(H7), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22),
 C24B(H24B), C25B(H25B), C26B(H26B), C27B(H27B), C28B(H28B), C28A(H28A),
 C27A(H27A), C26A(H26A), C25A(H25A), C24A(H24A)
6.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C13(H13A,H13B,
 H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C)
;
_shelx_res_checksum              19523
_olex2_submission_special_instructions 'No special instructions were received'