Reduction chemistry of neptunium cyclopentadienide complexes: from structure to understanding
Dutkiewicz, Michał S.; Apostolidis, Christos; Walter, Olaf; Arnold, Polly L.; Chem. Sci. 8 (2017) 2553–; doi:10.1039/C7SC00034K

data_1545183
_publ_section_title
;
 Reduction chemistry of neptunium cyclopentadienide complexes: from
 structure to understanding
;
_journal_issue                   4
_journal_name_full               'Chem. Sci.'
_journal_page_first              2553
_journal_paper_doi               10.1039/C7SC00034K
_journal_volume                  8
_journal_year                    2017
_chemical_formula_sum            'C15 H15 Np'
_chemical_formula_weight         432.27
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           36
_space_group_name_Hall           'C 2c -2'
_space_group_name_H-M_alt        'C m c 21'
_symmetry_space_group_name_Hall  'C 2c -2'
_symmetry_space_group_name_H-M   'C m c 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2016-12-22 deposited with the CCDC.
2017-01-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.1208(6)
_cell_length_b                   8.7037(6)
_cell_length_c                   9.5917(5)
_cell_measurement_reflns_used    8809
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.63
_cell_measurement_theta_min      2.745
_cell_volume                     1178.85(11)
_computing_cell_refinement       'APEX II (Bruker, 2007)'
_computing_data_collection       'APEX II (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics
'XPMA (Zsolnai, 1996), ORTEP (Farrugia, 1997)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXs-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 66
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker Apex II Quazar'
_diffrn_measurement_method       'combined omega- and phi-scan'
_diffrn_radiation_source         'Microfocus Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0211
_diffrn_reflns_av_unetI/netI     0.0119
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10413
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.355
_diffrn_reflns_theta_min         2.749
_exptl_absorpt_coefficient_mu    8.782
_exptl_absorpt_correction_T_max  0.621
_exptl_absorpt_correction_T_min  0.424
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   (sadabs)
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.436
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       quader
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.133
_exptl_crystal_size_mid          0.103
_exptl_crystal_size_min          0.074
_refine_diff_density_max         1.045
_refine_diff_density_min         -1.123
_refine_diff_density_rms         0.103
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.47(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     116
_refine_ls_number_reflns         1483
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0145
_refine_ls_R_factor_gt           0.0141
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0170P)^2^+5.7968P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0355
_refine_ls_wR_factor_ref         0.0359
_reflns_Friedel_coverage         0.886
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.990
_reflns_number_gt                1464
_reflns_number_total             1483
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc00034k2.cif
_cod_data_source_block           mdit34z
_cod_depositor_comments
'Adding full bibliography for 1545181--1545185.cif.'
_cod_database_code               1545183
_shelx_estimated_absorpt_t_min   0.388
_shelx_estimated_absorpt_t_max   0.563
_shelxl_version_number           2013-2
_shelx_res_checksum              1779