#------------------------------------------------------------------------------
#$Date: 2017-04-05 12:30:44 +0300 (Wed, 05 Apr 2017) $
#$Revision: 195014 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/54/51/1545181.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1545181
loop_
_publ_author_name
'Dutkiewicz, Michał S.'
'Apostolidis, Christos'
'Walter, Olaf'
'Arnold, Polly L.'
_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            'C2.5 H2.5 Np0.12'
_chemical_formula_weight         62.17
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           121
_space_group_name_Hall           'I -4 2'
_space_group_name_H-M_alt        'I -4 2 m'
_symmetry_space_group_name_Hall  'I -4 2'
_symmetry_space_group_name_H-M   'I -4 2 m'
_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            16
_cell_length_a                   8.59800(10)
_cell_length_b                   8.59800(10)
_cell_length_c                   10.5541(2)
_cell_measurement_reflns_used    476
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.7
_cell_measurement_theta_min      3.24
_cell_volume                     780.22(2)
_computing_cell_refinement       'SMART (Siemens, 1997)'
_computing_data_collection       'SMART (Siemens, 1997)'
_computing_data_reduction        'SAINT (Siemens, 1997)'
_computing_molecular_graphics    'XPMA (Zsolnai, 1996), winray (Soltek, 1997)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 1.003
_diffrn_measurement_device_type  'Siemens SMART CCD 1000'
_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  0.0232
_diffrn_reflns_av_unetI/netI     0.0131
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 1.003
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4046
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.230
_diffrn_reflns_theta_min         3.056
_exptl_absorpt_coefficient_mu    6.650
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.786
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   (sadabs)
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.117
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             466
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.260
_refine_diff_density_min         -0.165
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details
;
 Flack x determined using 215 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.12(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     49
_refine_ls_number_reflns         530
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0083
_refine_ls_R_factor_gt           0.0083
_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/[σ²(Fo²)+(0.0106P)²]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0187
_refine_ls_wR_factor_ref         0.0187
_reflns_Friedel_coverage         0.683
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.991
_reflns_number_gt                530
_reflns_number_total             530
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7sc00034k2.cif
_cod_data_source_block           bk8
_cod_depositor_comments
'Adding full bibliography for 1545181--1545185.cif.'
_cod_original_formula_sum        'C2.50 H2.50 Np0.12'
_cod_database_code               1545181
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           2013-2
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x, y, -z'
'x, -y, -z'
'-y, -x, z'
'y, x, z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Np1 Np 1.0000 1.0000 1.0000 0.01753(7) Uani 1 8 d S T P
C1 C 0.7367(19) 1.1871(17) 1.0510(16) 0.053(6) Uani 0.5 1 d . . P
H1 H 0.6716 1.2073 0.9825 0.13(2) Uiso 0.5 1 calc R U P
C2 C 0.7253(15) 1.0613(14) 1.1363(11) 0.039(2) Uani 0.5 1 d . . P
H2 H 0.6523 0.9815 1.1348 0.13(2) Uiso 0.5 1 calc R U P
C3 C 0.8424(17) 1.080(2) 1.2210(11) 0.053(6) Uani 0.5 1 d . . P
H3 H 0.8615 1.0136 1.2885 0.13(2) Uiso 0.5 1 calc R U P
C4 C 0.929(2) 1.211(2) 1.1950(19) 0.093(11) Uani 0.5 1 d . . P
H4 H 1.0149 1.2475 1.2398 0.13(2) Uiso 0.5 1 calc R U P
C5 C 0.8632(18) 1.2746(13) 1.0889(18) 0.086(9) Uani 0.5 1 d . . P
H5 H 0.8983 1.3640 1.0484 0.13(2) Uiso 0.5 1 calc R U P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Np Np -11.4937 4.1493 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C3 Np1 C3 19.4(7) 7_775 .
C3 Np1 C3 134.6(4) 7_775 6_577
C3 Np1 C3 121.8(6) . 6_577
C3 Np1 C3 151.2(7) 7_775 4_757
C3 Np1 C3 134.6(4) . 4_757
C3 Np1 C3 19.4(7) 6_577 4_757
C3 Np1 C3 62.6(6) 7_775 2_775
C3 Np1 C3 66.2(6) . 2_775
C3 Np1 C3 151.2(7) 6_577 2_775
C3 Np1 C3 134.6(4) 4_757 2_775
C3 Np1 C3 66.2(6) 7_775 8
C3 Np1 C3 62.6(6) . 8
C3 Np1 C3 134.6(4) 6_577 8
C3 Np1 C3 121.8(6) 4_757 8
C3 Np1 C3 19.4(7) 2_775 8
C3 Np1 C3 134.6(4) 7_775 5_757
C3 Np1 C3 151.2(7) . 5_757
C3 Np1 C3 66.2(6) 6_577 5_757
C3 Np1 C3 62.6(6) 4_757 5_757
C3 Np1 C3 121.8(6) 2_775 5_757
C3 Np1 C3 134.6(4) 8 5_757
C3 Np1 C3 121.8(6) 7_775 3_577
C3 Np1 C3 134.6(4) . 3_577
C3 Np1 C3 62.6(6) 6_577 3_577
C3 Np1 C3 66.2(6) 4_757 3_577
C3 Np1 C3 134.6(4) 2_775 3_577
C3 Np1 C3 151.2(7) 8 3_577
C3 Np1 C3 19.4(7) 5_757 3_577
C3 Np1 C5 106.0(5) 7_775 4_757
C3 Np1 C5 88.6(4) . 4_757
C3 Np1 C5 37.3(5) 6_577 4_757
C3 Np1 C5 46.0(5) 4_757 4_757
C3 Np1 C5 125.9(5) 2_775 4_757
C3 Np1 C5 106.6(5) 8 4_757
C3 Np1 C5 103.5(5) 5_757 4_757
C3 Np1 C5 97.6(5) 3_577 4_757
C3 Np1 C5 125.9(5) 7_775 6_577
C3 Np1 C5 106.6(5) . 6_577
C3 Np1 C5 46.0(5) 6_577 6_577
C3 Np1 C5 37.3(5) 4_757 6_577
C3 Np1 C5 106.0(5) 2_775 6_577
C3 Np1 C5 88.6(4) 8 6_577
C3 Np1 C5 97.6(5) 5_757 6_577
C3 Np1 C5 103.5(5) 3_577 6_577
C5 Np1 C5 34.8(6) 4_757 6_577
C3 Np1 C5 106.6(5) 7_775 3_577
C3 Np1 C5 125.9(5) . 3_577
C3 Np1 C5 103.5(5) 6_577 3_577
C3 Np1 C5 97.6(5) 4_757 3_577
C3 Np1 C5 88.6(4) 2_775 3_577
C3 Np1 C5 106.0(5) 8 3_577
C3 Np1 C5 37.3(5) 5_757 3_577
C3 Np1 C5 46.0(5) 3_577 3_577
C5 Np1 C5 140.8(8) 4_757 3_577
C5 Np1 C5 126.6(8) 6_577 3_577
C3 Np1 C5 88.6(4) 7_775 5_757
C3 Np1 C5 106.0(5) . 5_757
C3 Np1 C5 97.6(5) 6_577 5_757
C3 Np1 C5 103.5(5) 4_757 5_757
C3 Np1 C5 106.6(5) 2_775 5_757
C3 Np1 C5 125.9(5) 8 5_757
C3 Np1 C5 46.0(5) 5_757 5_757
C3 Np1 C5 37.3(5) 3_577 5_757
C5 Np1 C5 126.6(8) 4_757 5_757
C5 Np1 C5 140.8(8) 6_577 5_757
C5 Np1 C5 34.8(6) 3_577 5_757
C5 C1 C2 106.7(16) . .
C5 C1 Np1 74.6(11) . .
C2 C1 Np1 75.0(9) . .
C3 C2 C1 106.0(13) . .
C3 C2 Np1 74.7(9) . .
C1 C2 Np1 76.1(9) . .
C2 C3 C4 111.8(18) . .
C2 C3 Np1 77.3(8) . .
C4 C3 Np1 76.7(11) . .
C5 C4 C3 105.3(15) . .
C5 C4 Np1 75.5(9) . .
C3 C4 Np1 74.8(11) . .
C4 C5 C1 110.2(12) . .
C4 C5 Np1 76.2(8) . .
C1 C5 Np1 77.0(11) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Np1 C3 2.785(13) 7_775
Np1 C3 2.785(13) .
Np1 C3 2.785(13) 6_577
Np1 C3 2.785(13) 4_757
Np1 C3 2.785(13) 2_775
Np1 C3 2.785(13) 8
Np1 C3 2.785(13) 5_757
Np1 C3 2.785(13) 3_577
Np1 C5 2.800(12) 4_757
Np1 C5 2.800(12) 6_577
Np1 C5 2.800(12) 3_577
Np1 C5 2.800(12) 5_757
C1 C5 1.38(2) .
C1 C2 1.411(19) .
C2 C3 1.36(2) .
C3 C4 1.37(2) .
C4 C5 1.37(3) .
