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_7046983
_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_absolute_configuration ad
_chemical_formula_moiety         'C58 H72 Cu2 N4 O4, 2(C7 H8)'
_chemical_formula_sum            'C72 H88 Cu2 N4 O4'
_chemical_formula_weight         1200.54
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-12-01
_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                90
_cell_angle_beta                 108.617(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.2710(5)
_cell_length_b                   25.1487(10)
_cell_length_c                   11.9113(5)
_cell_measurement_reflns_used    9721
_cell_measurement_temperature    100
_cell_measurement_theta_max      72.00
_cell_measurement_theta_min      4.29
_cell_volume                     3199.6(2)
_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      100
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.963
_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  0.0219
_diffrn_reflns_av_unetI/netI     0.0191
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            43734
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.174
_diffrn_reflns_theta_min         4.139
_diffrn_source                   'Microfocus Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.211
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.6526
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/2 (Bruker,2014/2) was used for absorption correction. wR2(int) was 0.1355 before and 0.0333 after correction. The Ratio of minimum to maximum transmission is 0.8660. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_description       block
_exptl_crystal_F_000             1276
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.335
_refine_diff_density_min         -0.288
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.444(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     823
_refine_ls_number_reflns         12091
_refine_ls_number_restraints     272
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0264
_refine_ls_R_factor_gt           0.0262
_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^)+(0.0496P)^2^+0.7289P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0709
_refine_ls_wR_factor_ref         0.0712
_reflns_Friedel_coverage         0.957
_reflns_Friedel_fraction_full    0.977
_reflns_Friedel_fraction_max     0.968
_reflns_number_gt                12019
_reflns_number_total             12091
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02140f2.cif
_cod_data_source_block           comp_11b
_cod_depositor_comments
'Adding full bibliography for 7046963--7046983.cif.'
_cod_database_code               7046983
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.931
_shelx_estimated_absorpt_t_min   0.868
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.556(14)
 0.444(14)
2. 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
3. Restrained distances
 C67A-C69A \\sim C68A-C70A \\sim C69A-C71A \\sim C70A-C72A \\sim C71A-C67A
\\sim C72A-C68A \\sim C67A-
 C69B \\sim C68B-C70B \\sim C69B-C71B \\sim C70B-C72B \\sim C71B-C67A \\sim
C72B-C68B
 with sigma of 0.02
 C67A-C68A \\sim C68A-C69A \\sim C69A-C70A \\sim C70A-C71A \\sim C71A-C72A
\\sim C72A-C67A \\sim C67B-
 C68B \\sim C68B-C69B \\sim C69B-C70B \\sim C70B-C71B \\sim C71B-C72B \\sim
C72B-C67B
 with sigma of 0.001
 C66A-C72A \\sim C66A-C68A \\sim C66B-C72B \\sim C66B-C68B
 with sigma of 0.02
 C67A-C66A \\sim C67B-C66B
 with sigma of 0.001
4. 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
5. Rigid body (RIGU) restrains
 C66A, C67A, C68A, C69A, C70A, C71A, C72A, C67B, C66B, C68B, C69B, C70B, C71B,
 C72B
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
6. Others
 Sof(C66A)=Sof(H66a)=Sof(H66b)=Sof(H66c)=Sof(C67A)=Sof(C68A)=Sof(H68A)=
 Sof(C69A)=Sof(H69A)=Sof(C70A)=Sof(H70A)=Sof(C71A)=Sof(H71A)=Sof(C72A)=
 Sof(H72A)=1-FVAR(1)
 Sof(C67B)=Sof(C66B)=Sof(H66d)=Sof(H66e)=Sof(H66f)=Sof(C68B)=Sof(H68B)=
 Sof(C69B)=Sof(H69B)=Sof(C70B)=Sof(H70B)=Sof(C71B)=Sof(H71B)=Sof(C72B)=
 Sof(H72B)=FVAR(1)
7.a Secondary CH2 refined with riding coordinates:
 C47(H47a,H47b), C53(H53a,H53b)
7.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C5(H5), C18(H18), C19(H19), C20(H20), C24(H24), C26(H26),
 C28(H28), C41(H41), C42(H42), C43(H43), C49(H49), C50(H50), C51(H51), C52(H52),
  C55(H55), C56(H56), C57(H57), C58(H58), C61(H61), C62(H62), C63(H63),
 C64(H64), C65(H65), C68A(H68A), C69A(H69A), C70A(H70A), C71A(H71A), C72A(H72A),
  C68B(H68B), C69B(H69B), C70B(H70B), C71B(H71B), C72B(H72B)
7.c 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), C22(H22a,H22b,H22c), C23(H23a,
 H23b,H23c), C32(H32a,H32b,H32c), C33(H33a,H33b,H33c), C34(H34a,H34b,H34c),
 C36(H36a,H36b,H36c), C37(H37a,H37b,H37c), C38(H38a,H38b,H38c), C45(H45a,H45b,
 H45c), C46(H46a,H46b,H46c), C59(H59a,H59b,H59c), C66A(H66a,H66b,H66c),
 C66B(H66d,H66e,H66f)
;
_shelx_res_checksum              70476
_olex2_submission_special_instructions 'No special instructions were received'