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_7046969
_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         '2(C28 H34 Cu N2 O2), C7 H8'
_chemical_formula_sum            'C63 H76 Cu2 N4 O4'
_chemical_formula_weight         1080.35
_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             2017-12-01
_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                102.745(2)
_cell_angle_beta                 90.632(2)
_cell_angle_gamma                90.424(2)
_cell_formula_units_Z            2
_cell_length_a                   11.8306(4)
_cell_length_b                   13.9522(5)
_cell_length_c                   17.0501(6)
_cell_measurement_reflns_used    9851
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      71.79
_cell_measurement_theta_min      3.72
_cell_volume                     2744.69(17)
_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 0.975
_diffrn_measured_fraction_theta_max 0.966
_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  0.1204
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10437
_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         72.117
_diffrn_reflns_theta_min         2.657
_diffrn_source                   'Microfocus Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.353
_exptl_absorpt_correction_T_max  0.7535
_exptl_absorpt_correction_T_min  0.6717
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0773 before and 0.0586 after correction.
 The Ratio of minimum to maximum transmission is 0.85.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 98116 reflections, Rint = 0.1204
 (43258 with I > 3sig(I), Rint = 0.1226)
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_description       block
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.307
_refine_diff_density_min         -0.656
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     736
_refine_ls_number_reflns         10437
_refine_ls_number_restraints     229
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0600
_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^)+(0.1150P)^2^+2.0270P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1638
_refine_ls_wR_factor_ref         0.1658
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9883
_reflns_number_total             10437
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02140f2.cif
_cod_data_source_block           comp_8b
_cod_depositor_comments
'Adding full bibliography for 7046963--7046983.cif.'
_cod_database_code               7046969
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.900
_shelx_estimated_absorpt_t_min   0.877
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.8781(19)
 0.1219(19)
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
 C64-C70 \\sim C64-C66 \\sim C57-C59 \\sim C57-C63
 with sigma of 0.02
 C64-C65 \\sim C57-C58
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1A with sigma of 0.01 and sigma
for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 C57, C58, C59, C60, C61, C62, C63, C64, C65, C66, C67, C68, C69, C70
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Same fragment restrains
{C59, C60, C61, C62, C63, C58} sigma for 1-2: 0.02, 1-3: 0.04
{C58, C63, C62, C61, C60, C59} sigma for 1-2: 0.02, 1-3: 0.04
{C65, C66, C67, C68, C69, C70} sigma for 1-2: 0.02, 1-3: 0.04
as
{C58, C59, C60, C61, C62, C63}
{C66, C67, C68, C69, C70, C65} sigma for 1-2: 0.02, 1-3: 0.04
{C65, C70, C69, C68, C67, C66} sigma for 1-2: 0.02, 1-3: 0.04
as
{C65, C66, C67, C68, C69, C70}
7. Others
 Fixed Sof: C57(0.5) H57A(0.5) H57B(0.5) H57C(0.5) C58(0.5) C59(0.5) H59(0.5)
 C60(0.5) H60(0.5) C61(0.5) H61(0.5) C62(0.5) H62(0.5) C63(0.5) H63(0.5)
 C64(0.5) H64A(0.5) H64B(0.5) H64C(0.5) C65(0.5) C66(0.5) H66(0.5) C67(0.5)
 H67(0.5) C68(0.5) H68(0.5) C69(0.5) H69(0.5) C70(0.5) H70(0.5)
8.a Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C23(H23A,H23B), C44(H44A,H44B), C51(H51A,H51B)
8.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C5(H5), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22),
 C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C31(H31), C33(H33), C46(H46),
  C47(H47), C48(H48), C49(H49), C50(H50), C53(H53), C54(H54), C55(H55),
 C56(H56), C59(H59), C60(H60), C61(H61), C62(H62), C63(H63), C66(H66), C67(H67),
  C68(H68), C69(H69), C70(H70)
8.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), C37(H37A,H37B,H37C), C38(H38A,
 H38B,H38C), C39(H39A,H39B,H39C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C),
 C43(H43A,H43B,H43C), C57(H57A,H57B,H57C), C64(H64A,H64B,H64C)
;
_shelx_res_checksum              2585
_olex2_submission_special_instructions 'No special instructions were received'