Controlling uranyl oxo group interactions to group 14 elements using polypyrrolic Schiff-base macrocyclic ligands.
Bell, Nicola L.; Arnold, Polly L.; Love, Jason B.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 15902–15909; doi:10.1039/c6dt01948j

data_7039739
_publ_section_title
;
 Controlling uranyl oxo group interactions to group 14 elements using
 polypyrrolic Schiff-base macrocyclic ligands.
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15902
_journal_page_last               15909
_journal_paper_doi               10.1039/c6dt01948j
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C52 H50 N10 O2 Pb U'
_chemical_formula_sum            'C52 H50 N10 O2 Pb U'
_chemical_formula_weight         1292.24
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-04-07
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-06-17 deposited with the CCDC.
2016-06-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8424(3)
_cell_length_b                   15.8907(3)
_cell_length_c                   33.2881(8)
_cell_measurement_reflns_used    10887
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      20.4980
_cell_measurement_theta_min      2.9240
_cell_volume                     5735.3(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_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   24.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.3089  -99.0000  -30.0000 49

  2 omega  -25.00   24.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.3089  -99.0000 -180.0000 49

  3 omega  -91.00  -34.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.3089 -179.0000  120.0000 57

  4 omega  -35.00   52.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.3089   57.0000  -60.0000 87

  5 omega  -25.00   24.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.3089  -99.0000    0.0000 49

  6 omega  -20.00   90.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.8714   19.0000   30.0000 110

  7 omega   -1.00   86.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.8714   57.0000  150.0000 87

  8 omega  -20.00   90.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.8714   19.0000   90.0000 110

  9 omega  -74.00    0.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.3089  129.0000   84.0083 74

 10 omega   -1.00   86.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.8714   57.0000 -120.0000 87

 11 omega  -18.00   63.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.8714 -107.0000   -6.2344 81

 12 omega   -1.00   86.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.8714   57.0000  -60.0000 87

 13 omega  -51.00   36.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.8714  -57.0000   30.0000 87
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0176164000
_diffrn_orient_matrix_UB_12      -0.0076983000
_diffrn_orient_matrix_UB_13      0.0201885000
_diffrn_orient_matrix_UB_21      -0.0272044000
_diffrn_orient_matrix_UB_22      -0.0386882000
_diffrn_orient_matrix_UB_23      -0.0058790000
_diffrn_orient_matrix_UB_31      0.0568278000
_diffrn_orient_matrix_UB_32      -0.0208914000
_diffrn_orient_matrix_UB_33      0.0034420000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1807
_diffrn_reflns_av_unetI/netI     0.1087
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_number            11715
_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         26.372
_diffrn_reflns_theta_min         2.841
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.795
_exptl_absorpt_correction_T_max  0.772
_exptl_absorpt_correction_T_min  0.522
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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_density_diffrn    1.497
_exptl_crystal_F_000             2488
_exptl_crystal_size_max          0.1237
_exptl_crystal_size_mid          0.1188
_exptl_crystal_size_min          0.0469
_platon_squeeze_details
;
;
_refine_diff_density_max         2.589
_refine_diff_density_min         -1.257
_refine_diff_density_rms         0.186
_refine_ls_abs_structure_details
;
 Flack x determined using 2540 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.013(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     591
_refine_ls_number_reflns         11715
_refine_ls_number_restraints     507
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.1163
_refine_ls_R_factor_gt           0.0828
_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^)+(0.0622P)^2^+28.3352P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1471
_refine_ls_wR_factor_ref         0.1576
_reflns_Friedel_coverage         0.807
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                8552
_reflns_number_total             11715
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt01948j2.cif
_cod_data_source_block           UO2PbLMepy
_cod_depositor_comments
'Adding full bibliography for 7039733--7039741.cif.'
_cod_database_code               7039739
_chemical_oxdiff_formula         'C60 H100 N8 U O2 Pb'
_reflns_odcompleteness_completeness 99.72
_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. Uiso/Uaniso restraints and constraints
N00A \\sim N00G \\sim C00H \\sim C010: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
N005 \\sim C00S \\sim C00X \\sim C00Y \\sim C00Z \\sim C016: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
N00V \\sim C01T \\sim C01O \\sim C027 \\sim C01I \\sim C013: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C00T \\sim C00Y \\sim C01P: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
N00A \\sim C00S \\sim C01C: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
N007 \\sim C00M \\sim C017 \\sim C01H \\sim C01J: within 1.7A with sigma of
0.04 and sigma for terminal atoms of 0.08
N006 \\sim C00E \\sim N00I \\sim C00J \\sim C00W \\sim C01A \\sim C01E \\sim
C01L: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C00E \\sim C01E \\sim N00I: within 1.7A with sigma of 0.02 and sigma for
terminal atoms of 0.04
N008 \\sim C00D \\sim C00K \\sim C012 \\sim C00N: within 1.7A with sigma of
0.01 and sigma for terminal atoms of 0.02
C019 \\sim C00O \\sim C010 \\sim C00H \\sim C00L \\sim C00U: within 1.7A with
sigma of 0.02 and sigma for terminal atoms of 0.04
3. Rigid body (RIGU) restrains
 N00A, N00G, C00H, C010
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N005, C00S, C00X, C00Y, C00Z, C016
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N00V, C01T, C01O, C027, C01I, C013
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C00T, C00Y, C01P
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N00A, C00S, C01C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N007, C00M, C017, C01H, C01J
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N006, C00E, N00I, C00J, C00W, C01A, C01E, C01L
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N00I, C00E, C01E
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 N008, C00D, C00K, C012, C00N
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C00O, C010, C00H, C00L, C00U, C019
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4.a Aromatic/amide H refined with riding coordinates:
 C00B(H00B), C00F(H00F), C00J(H00J), C00K(H00K), C00L(H00L), C00O(H00O),
 C00Q(H00Q), C01T(H01T), C01O(H01O), C027(H027), C01I(H01I), C013(H013),
 C00Z(H00Z), C011(H011), C012(H012), C015(H015), C016(H016), C018(H018),
 C01A(H01D), C01B(H01E), C01C(H01F), C01F(H01K), C01H(H01P), C01J(H01Q),
 C01M(H01R), C01V(H0AA)
4.b Fitted hexagon refined as free rotating group:
 N00V(C01T,C01O,C027,C01I,C013)
4.c Idealised Me refined as rotating group:
 C00T(H00A,H00C,H00D), C014(H01A,H01B,H01C), C01D(H01G,H01H,H01J), C01G(H01L,
 H01M,H01N), C01N(H01S,H01U,H01V), C01P(H01W,H01X,H01Y), C01Q(H01Z,H,HA),
 C01R(H01,HB,HC)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'