Magnesium amino-bis(phenolato) complexes for the ring-opening polymerization of rac-lactide.
Devaine-Pressing, Katalin; Lehr, Joshua H.; Pratt, Michelle E.; Dawe, Louise N.; Sarjeant, Amy A.; Kozak, Christopher M.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 12365–12375; doi:10.1039/c5dt00236b

data_7034457
_publ_section_title
;
 Magnesium amino-bis(phenolato) complexes for the ring-opening
 polymerization of rac-lactide.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12365
_journal_page_last               12375
_journal_paper_doi               10.1039/c5dt00236b
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C56 H84 Mg2 N4 O4'
_chemical_formula_sum            'C56 H84 Mg2 N4 O4'
_chemical_formula_weight         925.89
_chemical_name_systematic        {Mg[O2NN]BuMe}2
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-02-26
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-02-27 deposited with the CCDC.
2015-03-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.998(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.345(14)
_cell_length_b                   9.706(5)
_cell_length_c                   25.551(12)
_cell_measurement_reflns_used    1069
_cell_measurement_temperature    163(2)
_cell_measurement_theta_max      21.44
_cell_measurement_theta_min      2.27
_cell_volume                     7102(6)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      163(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Rigaku Saturn70 CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0748
_diffrn_reflns_av_unetI/netI     0.0820
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            31988
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.438
_diffrn_reflns_theta_min         2.216
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.070
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4681
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/2 (Bruker,2014/2) was used for absorption correction.
wR2(int) was 0.0914 before and 0.0699 after correction.
The Ratio of minimum to maximum transmission is 0.6280.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    0.866
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2016
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Toluene'
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.409
_refine_diff_density_min         -0.379
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         7246
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.1222
_refine_ls_R_factor_gt           0.0784
_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^)+(0.1444P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2128
_refine_ls_wR_factor_ref         0.2416
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3982
_reflns_number_total             7246
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt00236b2.cif
_cod_data_source_block           ccent
_cod_depositor_comments          'Adding full bibliography for 7034457.cif.'
_cod_database_code               7034457
_shelxl_version_number           2013-4
_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
 C29-C25 \\sim C26-C25 \\sim C30-C25 \\sim C27-C25 \\sim C31-C25 \\sim C28-C25
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C31, C28, C29, C26, C30, C27
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(H29C)=Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=
 Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(H31C)=1-FVAR(1)
 Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(H27C)=
 Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C15(H15A,H15B), C16(H16A,H16B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C10(H10), C12(H12)
5.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,
 H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C),
 C30(H30A,H30B,H30C), C31(H31A,H31B,H31C)
;
_smtbx_masks_special_details
;
The OLEX2 solvent masking routine was applied to recover 56.6 electrons per 
unit cell in two voids. An area of disperse electron density appeared to be 
present prior to the solvent masking, however, a good point atom model could 
not be achieved for this, and the content was not accounted for in the formula 
(or resulting intensive properties). The application of the solvent mask gave 
a good improvement in the data statistics and allowed for a full anisotropic 
refinement of the framework structure.
;
_shelx_res_checksum              16899
_olex2_submission_special_instructions 'No special instructions were received'