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_7046976
_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         'C30 H24 Cl4 Cu N2 O2, C7 H8'
_chemical_formula_sum            'C37 H32 Cl4 Cu N2 O2'
_chemical_formula_weight         741.98
_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             2018-04-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.03 svn.r3497 for OlexSys, GUI svn.r5486)
;
_audit_update_record
;
2018-05-24 deposited with the CCDC.
2018-07-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.6030(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.0291(3)
_cell_length_b                   9.5222(3)
_cell_length_c                   16.5393(5)
_cell_measurement_reflns_used    9651
_cell_measurement_temperature    150
_cell_measurement_theta_max      60.65
_cell_measurement_theta_min      3.51
_cell_volume                     1725.46(9)
_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
_diffrn_detector_area_resol_mean 10.24
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.964
_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  0.0302
_diffrn_reflns_av_unetI/netI     0.0190
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            87742
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        53.000
_diffrn_reflns_theta_max         60.710
_diffrn_reflns_theta_min         2.340
_diffrn_source                   'Metal Jet'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.467
_exptl_absorpt_correction_T_max  0.7519
_exptl_absorpt_correction_T_min  0.5046
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/2 (Bruker,2014/2) was used for absorption correction. wR2(int) was 0.1453 before and 0.0878 after correction. The Ratio of minimum to maximum transmission is 0.6711. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_description       block
_exptl_crystal_F_000             762
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.239
_refine_diff_density_min         -0.556
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   -0.011(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     486
_refine_ls_number_reflns         6152
_refine_ls_number_restraints     251
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0251
_refine_ls_R_factor_gt           0.0249
_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^)+(0.0460P)^2^+0.1991P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0661
_refine_ls_wR_factor_ref         0.0664
_reflns_Friedel_coverage         0.882
_reflns_Friedel_fraction_full    0.969
_reflns_Friedel_fraction_max     0.961
_reflns_number_gt                6122
_reflns_number_total             6152
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02140f2.cif
_cod_data_source_block           comp_15c
_cod_depositor_comments
'Adding full bibliography for 7046963--7046983.cif.'
_cod_database_code               7046976
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.639
_shelx_estimated_absorpt_t_min   0.331
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 1.011(3)
 -0.011(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C32A-C33A \\sim C33A-C34A \\sim C34A-C35A \\sim C35A-C36A \\sim C36A-C37A
\\sim C37A-C32A \\sim C32B-
 C33B \\sim C33B-C34B \\sim C34B-C35B \\sim C35B-C36B \\sim C36B-C37B \\sim
C37B-C32B
 with sigma of 0.001
 C32A-C34A \\sim C33A-C35A \\sim C34A-C36A \\sim C35A-C37A \\sim C36A-C32A
\\sim C32B-C34B \\sim C33B-
 C35B \\sim C34B-C36B \\sim C35B-C37B \\sim C36B-C32B
 with sigma of 0.02
 C31A-C32A \\sim C31B-C32B
 with sigma of 0.001
 C31A-C33A \\sim C31B-C33B \\sim C31A-C37A \\sim C31B-C37B
 with sigma of 0.02
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
 C31A, C32A, C33A, C34A, C35A, C36A, C37A, C31B, C32B, C33B, C34B, C35B, C36B,
 C37B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
6. Others
 Sof(C32A)=Sof(C31A)=Sof(H31a)=Sof(H31b)=Sof(H31c)=Sof(C37A)=Sof(H37A)=
 Sof(C36A)=Sof(H36A)=Sof(C35A)=Sof(H35A)=Sof(C34A)=Sof(H34A)=Sof(C33A)=
 Sof(H33A)=1-FVAR(1)
 Sof(C31B)=Sof(H31d)=Sof(H31e)=Sof(H31f)=Sof(C32B)=Sof(C33B)=Sof(H33B)=
 Sof(C34B)=Sof(H34B)=Sof(C35B)=Sof(H35B)=Sof(C36B)=Sof(H36B)=Sof(C37B)=
 Sof(H37B)=FVAR(1)
7.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C5(H5), C10(H10), C11(H11), C12(H12), C16(H16), C18(H18),
 C20(H20), C25(H25), C26(H26), C27(H27), C37A(H37A), C36A(H36A), C35A(H35A),
 C34A(H34A), C33A(H33A), C33B(H33B), C34B(H34B), C35B(H35B), C36B(H36B),
 C37B(H37B)
7.b Idealised Me refined as rotating group:
 C14(H14a,H14b,H14c), C15(H15a,H15b,H15c), C29(H29a,H29b,H29c), C30(H30a,H30b,
 H30c), C31A(H31a,H31b,H31c), C31B(H31d,H31e,H31f)
;
_shelx_res_checksum              5451
_olex2_submission_special_instructions 'No special instructions were received'