Exploring the reactivity of manganese(iii) complexes with diphenolate-diamino ligands in rac-lactide polymerization.
Daneshmand, Pargol; Schaper, Frank; Dalton transactions (Cambridge, England : 2003) 44 (2015) 20449–20458; doi:10.1039/c5dt03756e

data_7036989
_publ_section_title
;
 Exploring the reactivity of manganese(iii) complexes with
 diphenolate-diamino ligands in rac-lactide polymerization.
;
_journal_issue                   47
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              20449
_journal_page_last               20458
_journal_paper_doi               10.1039/c5dt03756e
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C38 H57 Mn N2 O4, C H4 O'
_chemical_formula_sum            'C39 H61 Mn N2 O5'
_chemical_formula_weight         692.83
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-08-06
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-09-24 deposited with the CCDC.
2015-10-29 downloaded from the CCDC.
;
_cell_angle_alpha                104.320(5)
_cell_angle_beta                 103.352(5)
_cell_angle_gamma                92.336(5)
_cell_formula_units_Z            2
_cell_length_a                   10.5736(8)
_cell_length_b                   12.2554(9)
_cell_length_c                   16.4321(13)
_cell_measurement_reflns_used    8033
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      57.50
_cell_measurement_theta_min      3.26
_cell_volume                     1996.6(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX 2 (Bruker, 2014)'
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.15
_diffrn_detector                 'CMOS Area detector'
_diffrn_detector_area_resol_mean 10.24
_diffrn_detector_type            'Bruker Photon 100 CMOS Detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker Venture Metaljet'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_collimation    'Focusing mirrors'
_diffrn_radiation_monochromator  'Helios MX Mirror Optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0785
_diffrn_reflns_av_unetI/netI     0.0866
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            33228
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         60.786
_diffrn_reflns_theta_min         3.255
_diffrn_source                   'Metal Jet'
_diffrn_source_target            Ga
_diffrn_source_type              'Gallium Liquid Metal Jet Source'
_exptl_absorpt_coefficient_mu    1.966
_exptl_absorpt_correction_T_max  0.7519
_exptl_absorpt_correction_T_min  0.5869
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/2 (Bruker,2014/2) was used for absorption correction.
wR2(int) was 0.1097 before and 0.0746 after correction.
The Ratio of minimum to maximum transmission is 0.7806.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.152
_exptl_crystal_description       fragment
_exptl_crystal_F_000             748
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.652
_refine_diff_density_min         -0.532
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         9145
_refine_ls_number_restraints     70
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.1346
_refine_ls_R_factor_gt           0.0734
_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^)+(0.1131P)^2^+0.2842P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1817
_refine_ls_wR_factor_ref         0.2160
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5223
_reflns_number_total             9145
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03756e2.cif
_cod_data_source_block           parg32
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 7036988--7036991.cif.
;
_cod_database_code               7036989
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.859
_shelx_estimated_absorpt_t_min   0.828
_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, All O(H) groups
2. Restrained distances
 O4-H4
 0.87 with sigma of 0.01
 C38-H4
 1.921934 with sigma of 0.02
 Mn1-H4
 2.882848 with sigma of 0.02
 C29A-C27 \\sim C30A-C27 \\sim C28A-C27 \\sim C28B-C27 \\sim C30B-C27 \\sim
C29B-C27
 with sigma of 0.01
 C29A-C30A \\sim C30A-C28A \\sim C28A-C29A \\sim C29B-C30B \\sim C30B-C28B
\\sim C28B-C29B
 with sigma of 0.02
3. Restrained planarity
 O3, O5, H5A, C39
 with sigma of 0.1
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 0.04
5. Rigid body (RIGU) restrains
 C27, C28A, C29A, C30A, C28B, C29B, C30B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C28B)=Sof(H28D)=Sof(H28E)=Sof(H28F)=Sof(C29B)=Sof(H29D)=Sof(H29E)=
 Sof(H29F)=Sof(C30B)=Sof(H30D)=Sof(H30E)=Sof(H30F)=1-FVAR(1)
 Sof(C28A)=Sof(H28A)=Sof(H28B)=Sof(H28C)=Sof(C29A)=Sof(H29A)=Sof(H29B)=
 Sof(H29C)=Sof(C30A)=Sof(H30A)=Sof(H30B)=Sof(H30C)=FVAR(1)
7.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C22(H22A,H22B), C31(H31A,H31B)
7.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C18(H18), C20(H20), C33(H33), C34(H34), C35(H35), C36(H36)
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), C24(H24A,H24B,H24C), C25(H25A,
 H25B,H25C), C26(H26A,H26B,H26C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C),
 C28A(H28A,H28B,H28C), C29A(H29A,H29B,H29C), C30A(H30A,H30B,H30C), C28B(H28D,
 H28E,H28F), C29B(H29D,H29E,H29F), C30B(H30D,H30E,H30F), C39(H39A,H39B,H39C)
7.d Idealised tetrahedral OH refined as rotating group:
 O5(H5A)
;
_shelx_res_checksum              86878
_olex2_submission_special_instructions 'No special instructions were received'