Ring opening polymerisation of lactide with uranium(iv) and cerium(iv) phosphinoaryloxide complexes
Sinclair, Fern; Hlina, Johann A.; Wells, Jordann A. L.; Shaver, Michael P.; Arnold, Polly L.; Dalton Trans.  (2017) –; doi:10.1039/C7DT02167D

data_7043887
_publ_section_title
;
 Ring opening polymerisation of lactide with uranium(iv) and cerium(iv)
 phosphinoaryloxide complexes
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02167D
_journal_year                    2017
_chemical_formula_moiety         'C92 H96 O4 P4 U, 2(C4 H8 O)'
_chemical_formula_sum            'C100 H112 O6 P4 U'
_chemical_formula_weight         1627.59
_chemical_properties_physical
', Air-sensitive,Moisture-sensitive,Oxygen-sensitive'
_space_group_crystal_system      tetragonal
_space_group_IT_number           118
_space_group_name_Hall           'P -4 -2n'
_space_group_name_H-M_alt        'P -4 n 2'
_symmetry_space_group_name_Hall  'P -4 -2n'
_symmetry_space_group_name_H-M   'P -4 n 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-06-30
_audit_creation_method
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Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-07-03 deposited with the CCDC.
2017-07-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.0127(3)
_cell_length_b                   14.0127(3)
_cell_length_c                   21.3415(4)
_cell_measurement_reflns_used    18224
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      29.9180
_cell_measurement_theta_min      3.7600
_cell_volume                     4190.53(15)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      170.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0521
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -96.00  -34.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -20.0768 -179.0000 -180.0000 62

  2 omega  -90.00   10.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -20.0768  -77.0000  -30.0000 100

  3 omega   34.00   98.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       21.7955  179.0000  -60.0000 64

  4 omega   32.00   98.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       21.7955 -179.0000 -150.0000 66

  5 omega  -51.00   95.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       21.7955    0.0000  120.0000 146

  6 omega  -89.00  -56.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -20.0768  -57.0000  150.0000 33
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0408892000
_diffrn_orient_matrix_UB_12      0.0295828000
_diffrn_orient_matrix_UB_13      0.0026944000
_diffrn_orient_matrix_UB_21      -0.0195355000
_diffrn_orient_matrix_UB_22      0.0317609000
_diffrn_orient_matrix_UB_23      -0.0224766000
_diffrn_orient_matrix_UB_31      -0.0225703000
_diffrn_orient_matrix_UB_32      0.0260501000
_diffrn_orient_matrix_UB_33      0.0243250000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0494
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            38298
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.482
_diffrn_reflns_theta_min         3.212
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.061
_exptl_absorpt_correction_T_max  0.707
_exptl_absorpt_correction_T_min  0.561
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light green'
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_description       trapezoid
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          1.0328
_exptl_crystal_size_mid          0.7638
_exptl_crystal_size_min          0.455
_refine_diff_density_max         0.647
_refine_diff_density_min         -0.573
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.149(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         4807
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0235
_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^)+(0.0177P)^2^+3.2036P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0495
_refine_ls_wR_factor_ref         0.0544
_reflns_Friedel_coverage         0.845
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                3800
_reflns_number_total             4807
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02167d2.cif
_cod_data_source_block           3
_cod_original_cell_volume        4190.5(2)
_cod_database_code               7043887
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C92 H96 U1 O4 P4'
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.851(7)
 0.149(7)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C9) = Uanis(C11)
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C19(H19),
 C20(H20), C21(H21), C22(H22), C23(H23)
4.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C)
;
_shelx_res_checksum              96004
_shelx_fab_checksum              88530
_olex2_submission_special_instructions 'No special instructions were received'