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_7039736
_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         'C66 H64 N8 O4 Sn U, C4 H8 O'
_chemical_formula_sum            'C70 H71 N8 O5 Sn U'
_chemical_formula_weight         1461.06
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-04-29
_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                 97.5479(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.4369(2)
_cell_length_b                   22.3418(4)
_cell_length_c                   24.1875(4)
_cell_measurement_reflns_used    29780
_cell_measurement_temperature    170
_cell_measurement_theta_max      28.0400
_cell_measurement_theta_min      3.0530
_cell_volume                     6126.86(19)
_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
_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 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  1  \w    -47.00  43.00   1.00   30.00    --   21.95 -57.00 -30.00   90
  2  \w     -8.00  92.00   1.00   30.00    --   21.95  77.00-150.00  100
  3  \w      1.00  91.00   1.00   30.00    --   21.95  57.00 -30.00   90
  4  \w    -50.00  47.00   1.00   30.00    --   21.95 -38.00  60.00   97
  5  \w     -8.00  92.00   1.00   30.00    --   21.95  77.00  90.00  100
  6  \w    -95.00 -34.00   1.00   30.00    --  -19.30-179.00-180.00   61
  7  \w    -95.00 -34.00   1.00   30.00    --  -19.30-179.00 -30.00   61
  8  \w      1.00  91.00   1.00   30.00    --   21.95  57.00  60.00   90
  9  \w      5.00  87.00   1.00   30.00    --   21.95-137.00  48.00   82
 10  \w      2.00  84.00   1.00   30.00    --   21.95-133.00-134.00   82
 11  \w    -47.00  43.00   1.00   30.00    --   21.95 -57.00-180.00   90
 12  \w     34.00  98.00   1.00   30.00    --   21.95 179.00   0.00   64
 13  \w     34.00  98.00   1.00   30.00    --   21.95 179.00 -60.00   64
 14  \w     -4.00  32.00   1.00   30.00    --   21.95  38.00-150.00   36
;
_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      -0.0585147000
_diffrn_orient_matrix_UB_12      0.0110521000
_diffrn_orient_matrix_UB_13      -0.0049626000
_diffrn_orient_matrix_UB_21      0.0020411000
_diffrn_orient_matrix_UB_22      -0.0013334000
_diffrn_orient_matrix_UB_23      -0.0291494000
_diffrn_orient_matrix_UB_31      -0.0220138000
_diffrn_orient_matrix_UB_32      -0.0297451000
_diffrn_orient_matrix_UB_33      -0.0005401000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0678
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            135432
_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         27.103
_diffrn_reflns_theta_min         2.939
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.106
_exptl_absorpt_correction_T_max  0.498
_exptl_absorpt_correction_T_min  0.307
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.42b (Rigaku Oxford Diffraction, 2015)
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            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.584
_exptl_crystal_description       block
_exptl_crystal_F_000             2916
_exptl_crystal_size_max          0.503
_exptl_crystal_size_mid          0.262
_exptl_crystal_size_min          0.246
_refine_diff_density_max         1.518
_refine_diff_density_min         -0.593
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.908
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     790
_refine_ls_number_reflns         13495
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      0.912
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0359
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1115
_refine_ls_wR_factor_ref         0.1232
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11216
_reflns_number_total             13495
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt01948j2.cif
_cod_data_source_block           UO2SnLAthf
_cod_depositor_comments
'Adding full bibliography for 7039733--7039741.cif.'
_cod_original_cell_volume        6126.84(19)
_cod_database_code               7039736
_chemical_oxdiff_formula         'C60 H70 U Sn N8 O3'
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.04
_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. Uiso/Uaniso restraints and constraints
C59 \\sim C60 \\sim C61 \\sim C62 \\sim O3: within 1.7A with sigma of 0.02 and
sigma for terminal atoms of 0.04
O5 \\sim C67 \\sim C68 \\sim C69 \\sim C70: within 1.7A with sigma of 0.02 and
sigma for terminal atoms of 0.04
3. Rigid body (RIGU) restrains
 C59, O3, C62, C61, C60
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O5, C67, C68, C69, C70
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Others
 Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=1-FVAR(1)
 Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C62(H62A,H62B), C65(H65A,H65B), C66(H66A,H66B), C33(H33A,H33B), C59(H59A,
 H59B), C63(H63A,H63B), C64(H64A,H64B), C31(H31A,H31B), C4(H4A,H4B), C60(H60A,
 H60B), C70(H70A,H70B), C61(H61A,H61B), C68(H68A,H68B), C67(H67A,H67B),
 C69(H69A,H69B), C2(H2A,H2B), C2A(H2AA,H2AB)
5.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C54(H54), C46(H46), C25(H25), C23(H23), C56(H56), C22(H22),
 C10(H10), C52(H52), C28(H28), C20(H20), C36(H36), C49(H49), C27(H27), C21(H21),
  C51(H51), C50(H50), C39(H39), C14(H14), C42(H42), C43(H43), C12(H12),
 C13(H13), C41(H41), C57(H57), C8(H8), C37(H37), C7(H7)
5.c Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C32(H32A,H32B,H32C), C5(H5A,H5B,H5C), C3(H3A,H3B,H3C),
 C3A(H3AA,H3AB,H3AC)
;
_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 1.398
_oxdiff_exptl_absorpt_empirical_full_min 0.731