A versatile precursor for non-aqueous neptunyl(V) chemistry
Roy Copping; Victor Mougel; Sebastien Petit; Christophe Den Auwer; Philippe Moisy; Marinella Mazzanti; Chem.Commun. 47 (2011) 5497–; doi:10.1039/c1cc11010a

data_7106378
_publ_section_title
;
 A versatile precursor for non-aqueous neptunyl(V) chemistry
;
_journal_name_full               Chem.Commun.
_journal_page_first              5497
_journal_paper_doi               10.1039/c1cc11010a
_journal_volume                  47
_journal_year                    2011
_chemical_formula_sum            'C35 H35 I2 K N7 Np O2'
_chemical_formula_weight         1115.60
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.6120(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.8718(11)
_cell_length_b                   19.2117(17)
_cell_length_c                   16.0401(14)
_cell_measurement_reflns_used    9875
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      53.602
_cell_measurement_theta_min      9.890
_cell_volume                     3898.7(6)
_computing_cell_refinement       'Bruker SAINT v7.34a'
_computing_data_collection       'Bruker APEX 2'
_computing_data_reduction        'Bruker SAINT v7.34a'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL & local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device_type
'Bruker Nonius Kappa APEX II CCD diffractometer'
_diffrn_measurement_method
;
\w rotation to cover a hemisphere of reciprocal space
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0197
_diffrn_reflns_av_sigmaI/netI    0.0163
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            32382
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.85
_diffrn_reflns_theta_min         4.91
_exptl_absorpt_coefficient_mu    4.395
_exptl_absorpt_correction_T_max  0.4735
_exptl_absorpt_correction_T_min  0.2173
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/1 Bruker AXS Madison WI USA'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.901
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.835
_refine_diff_density_min         -0.862
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         7878
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.0190
_refine_ls_R_factor_gt           0.0172
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0174P)^2^+2.6379P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0405
_refine_ls_wR_factor_ref         0.0410
_reflns_number_gt                7430
_reflns_number_total             7878
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc11010a.txt
_cod_data_source_block           rcmnp15abs
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7106378