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_7039738
_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 O3 Pb U'
_chemical_formula_sum            'C52 H50 N10 O3 Pb U'
_chemical_formula_weight         1308.24
_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             2016-04-28
_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                   13.4429(2)
_cell_length_b                   19.5975(3)
_cell_length_c                   21.9112(4)
_cell_measurement_reflns_used    19587
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      29.4250
_cell_measurement_theta_min      3.4610
_cell_volume                     5772.45(16)
_computing_cell_refinement       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_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
;
List of Runs (angles in degrees, time in seconds):

  1  \w    -25.00  22.00   1.00   17.50    --  -18.68 -99.00-120.00   47
  2  \w    -25.00  22.00   1.00   17.50    --  -18.68 -99.00-180.00   47
  3  \w    -87.00   0.00   1.00   17.50    --  -18.68 -57.00 -90.00   87
  4  \w     34.00  94.00   1.00   17.50    --   20.25 179.00-150.00   60
  5  \w    -48.00  39.00   1.00   17.50    --   20.25 -57.00   0.00   87
  6  \w      2.00  89.00   1.00   17.50    --   20.25  57.00 150.00   87
  7  \w      2.00  43.00   1.00   17.50    --   20.25  57.00  30.00   41
  8  \w    -50.00  43.00   1.00   17.50    --   20.25 -38.00-150.00   93
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0284663000
_diffrn_orient_matrix_UB_12      -0.0106843000
_diffrn_orient_matrix_UB_13      -0.0255068000
_diffrn_orient_matrix_UB_21      -0.0040073000
_diffrn_orient_matrix_UB_22      0.0343675000
_diffrn_orient_matrix_UB_23      -0.0098975000
_diffrn_orient_matrix_UB_31      0.0442451000
_diffrn_orient_matrix_UB_32      -0.0038543000
_diffrn_orient_matrix_UB_33      -0.0172987000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0613
_diffrn_reflns_av_unetI/netI     0.0498
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            68331
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         2.976
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.760
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50167
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.42b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_description       block
_exptl_crystal_F_000             2520
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.102
_refine_diff_density_max         3.430
_refine_diff_density_min         -2.325
_refine_diff_density_rms         0.131
_refine_ls_abs_structure_details
;
 Flack x determined using 4427 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.001(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     612
_refine_ls_number_reflns         13223
_refine_ls_number_restraints     132
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0388
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0266P)^2^+15.7017P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0791
_refine_ls_wR_factor_ref         0.0851
_reflns_Friedel_coverage         0.824
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                11200
_reflns_number_total             13223
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt01948j2.cif
_cod_data_source_block           UO2PbLMepyPY-O
_cod_depositor_comments
'Adding full bibliography for 7039733--7039741.cif.'
_cod_original_cell_volume        5772.42(16)
_cod_database_code               7039738
_chemical_oxdiff_formula         'C52 H50 N10 O3 U Pb'
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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
C11 \\sim C10 \\sim C9 \\sim C16 \\sim C15 \\sim C13: within 1.7A with sigma of
0.02 and sigma for terminal atoms of 0.04
C6 \\sim C7 \\sim N1 \\sim C4 \\sim C5: within 1.7A with sigma of 0.02 and
sigma for terminal atoms of 0.04
3. Rigid body (RIGU) restrains
 C10, C9, C16, C15, C13, C11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C10, C9, C16, C15, C13, C11
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C6, C7, N1, C4, C5
 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:
 C15(H15), C17(H17), C29(H29), C47(H47), C8(H8), C31(H31), C20(H20), C38(H38),
 C45(H45), C36(H36), C41(H41), C40(H40), C015(H015), C19(H19), C26(H26),
 C10(H10), C43(H43), C51(H51), C6(H6), C5(H5), C48(H48), C27(H27), C52(H52),
 C44(H44), C50(H50), C49(H49)
4.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C14(H14A,H14B,H14C), C24(H24A,H24B,H24C), C33(H33A,H33B,
 H33C), C2(H2A,H2B,H2C), C23(H23A,H23B,H23C), C35(H35A,H35B,H35C), C12(H12A,
 H12B,H12C)
;
_shelx_fab_checksum              37159
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.654
_oxdiff_exptl_absorpt_empirical_full_min 0.734
_platon_squeeze_void_probe_radius 1.20