Organometallic neptunium(III) complexes
Michal S. Dutkiewicz; Joy H. Farnaby; Christos Apostolidis; Eric Colineau; Olaf Walter; Nicola Magnani; Michael G. Gardiner; Jason B. Love; Nikolas Kaltsoyannis; Roberto Caciuffo; Polly L. Arnold; Nature Chemistry 8 (2016) 797–802; doi:10.1038/nchem.2520

data_1552012
_publ_section_title
;
 Organometallic neptunium(III) complexes
;
_journal_name_full               'Nature Chemistry'
_journal_page_first              797
_journal_page_last               802
_journal_paper_doi               10.1038/nchem.2520
_journal_volume                  8
_journal_year                    2016
_chemical_formula_moiety         'C44 H60 Cl4 N2 Np2 O3, 0.5(C4 H8 O)'
_chemical_formula_sum            'C46 H64 Cl4 N2 Np2 O3.5'
_chemical_formula_weight         1316.79
_chemical_name_systematic        Np2Cl4(L)(THF)3
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                75.1470(10)
_cell_angle_beta                 75.7320(10)
_cell_angle_gamma                84.3340(10)
_cell_formula_units_Z            2
_cell_length_a                   10.5639(7)
_cell_length_b                   13.6771(8)
_cell_length_c                   18.1083(11)
_cell_measurement_reflns_used    4594
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.99
_cell_measurement_theta_min      2.356
_cell_volume                     2449.2(3)
_computing_cell_refinement       'APEX II (Bruker, 2007)'
_computing_data_collection       'APEX II (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_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    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 66
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.888
_diffrn_measurement_device_type  'Bruker Apex II Quazar'
_diffrn_measurement_method       'combined omega- and phi-scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_av_unetI/netI     0.0788
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.888
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            21583
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.888
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.497
_diffrn_reflns_theta_min         1.541
_exptl_absorpt_coefficient_mu    4.478
_exptl_absorpt_correction_T_max  0.9357
_exptl_absorpt_correction_T_min  0.7041
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.786
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.084
_exptl_crystal_size_mid          0.065
_exptl_crystal_size_min          0.015
_refine_diff_density_max         1.773
_refine_diff_density_min         -1.603
_refine_diff_density_rms         0.208
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     549
_refine_ls_number_reflns         11029
_refine_ls_number_restraints     76
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0414
_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^)+(0.0434P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0871
_refine_ls_wR_factor_ref         0.0997
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7761
_reflns_number_total             11029
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            nchem.2520-s3.cif
_cod_data_source_block           mdit25
_cod_original_formula_sum        'C46 H64 Cl4 N2 Np2 O3.50'
_cod_database_code               1552012
_shelx_estimated_absorpt_t_max   0.936
_shelx_estimated_absorpt_t_min   0.705
_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. Rigid body (RIGU) restrains
 O4, C45, C46, C47, C48
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C10, C9, C8, C13, C12, C11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Same fragment restrains
{O1, C33, C34, C35, C36} sigma for 1-2: 0.02, 1-3: 0.02
as
{O4, C45, C46, C47, C48}
4. Others
 Fixed Sof: O4(0.5) C45(0.5) H45A(0.5) H45B(0.5) C46(0.5) H46A(0.5) H46B(0.5)
 C47(0.5) H47A(0.5) H47B(0.5) C48(0.5) H48B(0.5) H48A(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,
 H37B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B),
 C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B),
  C47(H47A,H47B), C48(H48B,H48A)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C9(H9), C10(H10), C11(H11), C13(H13), C18(H18), C19(H19),
 C25(H25), C26(H26), C27(H27), C29(H29)
5.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C),
 C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C31(H31A,H31B,H31C), C32(H32A,H32B,
 H32C)
;
_shelx_res_checksum              79614
_shelx_hkl_checksum              41324
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'