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_7043888
_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         'C72 H81 Ce O4 P3 Si, 2(C6 H14)'
_chemical_formula_sum            'C84 H109 Ce O4 P3 Si'
_chemical_formula_weight         1271.48
_chemical_properties_physical
', Air-sensitive,Moisture-sensitive,Oxygen-sensitive'
_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
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;
Olex2 1.2-beta
(compiled 2015.11.10 svn.r3248 for OlexSys, GUI svn.r5133)
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_audit_update_record
;
2017-07-03 deposited with the CCDC.
2017-07-14 downloaded from the CCDC.
;
_cell_angle_alpha                102.706(2)
_cell_angle_beta                 102.3247(19)
_cell_angle_gamma                93.444(2)
_cell_formula_units_Z            2
_cell_length_a                   11.9128(3)
_cell_length_b                   12.8140(4)
_cell_length_c                   25.3401(6)
_cell_measurement_reflns_used    16232
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      26.9100
_cell_measurement_theta_min      3.2760
_cell_volume                     3663.17(18)
_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
;
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)'
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_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      170(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1042
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -25.00   25.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9986  -99.0000    0.0000 50

  2 omega  -93.00  -34.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9986 -179.0000 -150.0000 59

  3 omega   -6.00   92.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       19.5767   38.0000 -180.0000 98

  4 omega  -51.00   50.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       19.5767  -77.0000 -150.0000 101

  5 omega  -53.00   64.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       19.5767  -19.0000  -30.0000 117

  6 omega  -25.00   25.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9986  -99.0000 -180.0000 50

  7 omega  -25.00    0.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       19.5767  -99.0000  150.0000 25

  8 omega   -6.00   92.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       19.5767   38.0000   90.0000 98

  9 omega    1.00   80.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       19.5767 -130.0000   49.5049 79

 10 omega   34.00   96.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       19.5767  179.0000 -150.0000 62

 11 omega   -2.00   88.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       19.5767   57.0000  -30.0000 90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0229569000
_diffrn_orient_matrix_UB_12      0.0487103000
_diffrn_orient_matrix_UB_13      -0.0030557000
_diffrn_orient_matrix_UB_21      -0.0529222000
_diffrn_orient_matrix_UB_22      -0.0296695000
_diffrn_orient_matrix_UB_23      -0.0162524000
_diffrn_orient_matrix_UB_31      -0.0208329000
_diffrn_orient_matrix_UB_32      0.0028157000
_diffrn_orient_matrix_UB_33      0.0244342000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0537
_diffrn_reflns_av_unetI/netI     0.0576
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_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       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            59812
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.918
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.745
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98535
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'translucent dark brown'
_exptl_crystal_density_diffrn    1.153
_exptl_crystal_description       block
_exptl_crystal_F_000             1324
_exptl_crystal_size_max          0.2134
_exptl_crystal_size_mid          0.0822
_exptl_crystal_size_min          0.0493
_refine_diff_density_max         0.565
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     745
_refine_ls_number_reflns         14943
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0382
_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^)+(0.0350P)^2^+0.5912P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0749
_refine_ls_wR_factor_ref         0.0797
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12208
_reflns_number_total             14943
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02167d2.cif
_cod_data_source_block           2
_cod_original_cell_volume        3663.17(16)
_cod_database_code               7043888
_chemical_oxdiff_formula         'C70 H70 O4 P3 Si Ce'
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C1AA(H1AA), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17),
 C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C26(H26), C28(H28), C36(H36),
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 C45(H45), C46(H46), C49(H49), C51(H51), C59(H59), C60(H60), C61(H61), C62(H62),
  C63(H63), C65(H65), C66(H66), C67(H67), C68(H68), C69(H69)
2.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C),
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 H34C), C53(H53A,H53B,H53C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C57(H57A,
 H57B,H57C), C70(H70A,H70B,H70C), C71(H71A,H71B,H71C), C72(H72A,H72B,H72C)
;
_shelx_fab_checksum              96929
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'