Inner-sphere vs. outer-sphere reduction of uranyl supported by a redox-active, donor-expanded dipyrrin.
Pankhurst, James R.; Bell, Nicola L.; Zegke, Markus; Platts, Lucy N.; Lamfsus, Carlos Alvarez; Maron, Laurent; Natrajan, Louise S.; Sproules, Stephen; Arnold, Polly L.; Love, Jason B.; Chemical science 8 (2017) 108–116; doi:10.1039/c6sc02912d

data_1544404
_publ_section_title
;
 Inner-sphere vs. outer-sphere reduction of uranyl supported by a
 redox-active, donor-expanded dipyrrin.
;
_journal_issue                   1
_journal_name_full               'Chemical science'
_journal_page_first              108
_journal_page_last               116
_journal_paper_doi               10.1039/c6sc02912d
_journal_volume                  8
_journal_year                    2017
_chemical_formula_sum            'C37 H36 Cl F5 N4 O2 U'
_chemical_formula_weight         937.18
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-01-11 deposited with the CCDC.
2016-10-12 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 91.1720(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.5647(2)
_cell_length_b                   8.42790(10)
_cell_length_c                   16.88590(10)
_cell_measurement_reflns_used    27275
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      75.8840
_cell_measurement_theta_min      5.2110
_cell_volume                     3495.14(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
;
_computing_molecular_graphics    MERCURY
_computing_publication_material  ORTEP
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    Patterson
_diffrn_ambient_temperature      119.96(13)
_diffrn_detector_area_resol_mean 5.1574
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_sigmaI/netI    0.0249
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            34748
_diffrn_reflns_theta_full        76.14
_diffrn_reflns_theta_max         76.14
_diffrn_reflns_theta_min         3.60
_exptl_absorpt_coefficient_mu    14.349
_exptl_absorpt_correction_T_max  0.871
_exptl_absorpt_correction_T_min  0.743
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.781
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.1059
_exptl_crystal_size_mid          0.0508
_exptl_crystal_size_min          0.0437
_refine_diff_density_max         3.811
_refine_diff_density_min         -0.855
_refine_diff_density_rms         0.119
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.021(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         7244
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0273
_refine_ls_R_factor_gt           0.0270
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0461P)^2^+11.6706P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0677
_refine_ls_wR_factor_ref         0.0680
_reflns_number_gt                7139
_reflns_number_total             7244
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c6sc02912d2.cif
_cod_data_source_block           jl4006_monoc_refinalized
_cod_depositor_comments
;Adding full bibliography for 1544404--1544406.cif.

 Adding full bibliography for 1544404--1544406.cif.
;
_cod_database_code               1544404