Neptunyl(VI) centred visible LMCT emission directly observable in the presence of uranyl(VI)
Sean D. Woodall; Adam N. Swinburne; Nidhu lal Banik; Andrew Kerridge; Poppy Di Pietro; Christian Adam; Peter Kaden; Louise S. Natrajan; Chem.Commun. 51 (2015) 5402–; doi:10.1039/C4cc08718F

data_7116776
_publ_section_title
;
 Neptunyl(VI) centred visible LMCT emission directly observable in the
 presence of uranyl(VI)
;
_journal_name_full               Chem.Commun.
_journal_page_first              5402
_journal_paper_doi               10.1039/C4cc08718F
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'C66 H55 N2 Np O7 P5'
_chemical_formula_sum            'C66 H55 N2 Np O7 P5'
_chemical_formula_weight         1379.97
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-11-25
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.21 svn.r3092 for OlexSys, GUI svn.r4949)
;
_audit_update_record
;
2014-12-13 deposited with the CCDC.
2014-12-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.6657(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.61157(19)
_cell_length_b                   16.5891(2)
_cell_length_c                   26.4952(4)
_cell_measurement_reflns_used    32360
_cell_measurement_temperature    150.03(18)
_cell_measurement_theta_max      28.5360
_cell_measurement_theta_min      3.2960
_cell_volume                     5980.19(14)
_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, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.03(18)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0714
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
  1 omega  -11.00   93.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       20.9454   77.0000   60.0000 104

  2 omega   -3.00   91.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       20.9454   57.0000    0.0000 94

  3 omega   -1.00   40.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       20.9454  -57.0000 -150.0000 41

  4 omega  -64.00   -2.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.1798  -77.0000  120.0000 62

  5 omega  -93.00    8.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.1798  -77.0000 -150.0000 101

  6 omega  -87.00  -62.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.1798  178.0000   90.0000 25

  7 omega  -29.00   29.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.1798   37.0000  -30.0000 58

  8 omega  -39.00  -10.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.1798   37.0000 -150.0000 29
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0193922000
_diffrn_orient_matrix_UB_12      -0.0286709000
_diffrn_orient_matrix_UB_13      0.0174704000
_diffrn_orient_matrix_UB_21      -0.0482609000
_diffrn_orient_matrix_UB_22      -0.0090203000
_diffrn_orient_matrix_UB_23      0.0077048000
_diffrn_orient_matrix_UB_31      -0.0039458000
_diffrn_orient_matrix_UB_32      -0.0304202000
_diffrn_orient_matrix_UB_33      -0.0187533000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            51286
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.045
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.927
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56834
_exptl_absorpt_correction_type   multi-scan
_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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.533
_exptl_crystal_description       block
_exptl_crystal_F_000             2756
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.884
_refine_diff_density_min         -1.090
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     730
_refine_ls_number_reflns         12137
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0265
_refine_ls_R_factor_gt           0.0231
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0172P)^2^+5.8268P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0510
_refine_ls_wR_factor_ref         0.0523
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11200
_reflns_number_total             12137
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc08718f2.cif
_cod_data_source_block           alsn37
_cod_original_cell_volume        5980.21(15)
_cod_database_code               7116776
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         Np1O6P4n2C48H40
_reflns_odcompleteness_completeness 99.41
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21),
  C22(H22), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29),
 C30(H30), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C38(H38), C39(H39),
  C40(H40), C41(H41), C42(H42), C44(H44), C45(H45), C46(H46), C47(H47),
 C48(H48), C50(H50), C51(H51), C52(H52), C53(H53), C54(H54), C56(H56), C57(H57),
  C58(H58), C59(H59), C60(H60), C62(H62), C63(H63), C64(H64), C65(H65), C66(H66)
;
_shelx_res_checksum              4620
_olex2_date_sample_data_collection 2013-06-26
_olex2_submission_special_instructions 'No special instructions were received'