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_1545182
_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            'C32 H35 K1.5 Np1.5 O0.5'
_chemical_formula_weight         841.75
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_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                 90.4150(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.6093(10)
_cell_length_b                   14.7125(10)
_cell_length_c                   9.0155(5)
_cell_measurement_reflns_used    7796
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.61
_cell_measurement_theta_min      2.26
_cell_volume                     2998.8(3)
_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 1.000
_diffrn_measured_fraction_theta_max 0.945
_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  0.0474
_diffrn_reflns_av_unetI/netI     0.0497
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            27617
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.923
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.568
_diffrn_reflns_theta_min         1.651
_exptl_absorpt_coefficient_mu    5.406
_exptl_absorpt_correction_T_max  0.902
_exptl_absorpt_correction_T_min  0.805
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            'intense red-brown'
_exptl_crystal_density_diffrn    1.864
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       quader
_exptl_crystal_F_000             1596
_exptl_crystal_size_max          0.044
_exptl_crystal_size_mid          0.032
_exptl_crystal_size_min          0.024
_refine_diff_density_max         1.304
_refine_diff_density_min         -0.868
_refine_diff_density_rms         0.173
_refine_ls_abs_structure_details
;
 Flack x determined using 2856 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.000(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         7071
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0330
_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^)+(0.0352P)^2^+13.1553P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0753
_refine_ls_wR_factor_ref         0.0783
_reflns_Friedel_coverage         0.882
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.900
_reflns_number_gt                6479
_reflns_number_total             7071
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc00034k2.cif
_cod_data_source_block           mdit67
_cod_depositor_comments
'Adding full bibliography for 1545181--1545185.cif.'
_cod_original_formula_sum        'C32 H35 K1.50 Np1.50 O0.50'
_cod_database_code               1545182
_shelx_estimated_absorpt_t_min   0.797
_shelx_estimated_absorpt_t_max   0.881
_shelxl_version_number           2013-2
_shelx_res_checksum              3924