#------------------------------------------------------------------------------
#$Date: 2016-04-05 20:33:09 +0300 (Tue, 05 Apr 2016) $
#$Revision: 181722 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/60/7036039.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_7036039
loop_
_publ_author_name
'Hinz, Alexander'
'Rothe, Julia'
'Schulz, Axel'
'Villinger, Alexander'
_publ_section_title
;
 Reduction of dichloro(diaza-phospha)stibanes - isolation of a
 donor-stabilized distibenium dication.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6044
_journal_page_last               6052
_journal_paper_doi               10.1039/c5dt02711j
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C96 H100 N4 P2 Sb2'
_chemical_formula_sum            'C96 H100 N4 P2 Sb2'
_chemical_formula_weight         1615.23
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           48
_space_group_name_Hall           '-P 2ab 2bc'
_space_group_name_H-M_alt        'P n n n'
_symmetry_space_group_name_Hall  '-P 2ab 2bc'
_symmetry_space_group_name_H-M   'P n n n :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-06-01 deposited with the CCDC.
2015-08-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.3403(5)
_cell_length_b                   15.7088(7)
_cell_length_c                   16.8844(6)
_cell_measurement_reflns_used    4828
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.71
_cell_measurement_theta_min      2.59
_cell_volume                     4068.8(3)
_computing_cell_refinement       'Bruker Apex V7.51A'
_computing_data_collection       'Bruker Apex V7.51A'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material  SHELXL-2013
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Apex Kappa II-CCD-diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0670
_diffrn_reflns_av_unetI/netI     0.0540
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            37272
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.498
_diffrn_reflns_theta_min         3.044
_exptl_absorpt_coefficient_mu    0.752
_exptl_absorpt_correction_T_max  0.7468
_exptl_absorpt_correction_T_min  0.6780
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_description       block
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.506
_refine_diff_density_min         -0.834
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         6776
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0883
_refine_ls_R_factor_gt           0.0419
_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)+(0.0385P)²+3.1647P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0865
_refine_ls_wR_factor_ref         0.1077
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4081
_reflns_number_total             6776
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5dt02711j2.cif
_cod_data_source_block           ah209a
_cod_depositor_comments
'Adding full bibliography for 7036034--7036039.cif.'
_cod_database_code               7036039
_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.
;
_shelx_estimated_absorpt_t_min   0.876
_shelx_estimated_absorpt_t_max   0.949
_shelxl_version_number           2013-4
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x+1/2, y, -z+1/2'
'x, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x-1/2, -y, z-1/2'
'-x, y-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
Sb1 Sb 0.2500 0.2500 0.67171(2) 0.02521(7) Uani 1 2 d S T P
P1 P 0.03110(6) 0.2500 0.7500 0.02265(17) Uani 1 2 d S T P
N1 N 0.09541(13) 0.24899(15) 0.67439(11) 0.0224(4) Uani 1 1 d . . .
C1 C 0.06156(16) 0.26241(16) 0.59634(14) 0.0241(5) Uani 1 1 d . . .
C2 C 0.07740(17) 0.20103(17) 0.53674(15) 0.0268(5) Uani 1 1 d . . .
C3 C 0.05557(19) 0.22040(19) 0.45875(16) 0.0325(6) Uani 1 1 d . . .
H3 H 0.0668 0.1797 0.4184 0.039 Uiso 1 1 calc R U .
C4 C 0.0180(2) 0.2972(2) 0.43858(16) 0.0382(7) Uani 1 1 d . . .
H4 H 0.0058 0.3100 0.3847 0.046 Uiso 1 1 calc R U .
C5 C -0.0015(2) 0.35498(19) 0.49716(16) 0.0358(6) Uani 1 1 d . . .
H5 H -0.0289 0.4072 0.4834 0.043 Uiso 1 1 calc R U .
C6 C 0.01817(17) 0.33838(18) 0.57658(15) 0.0283(5) Uani 1 1 d . . .
C7 C 0.10779(18) 0.11203(17) 0.55189(14) 0.0271(5) Uani 1 1 d . . .
C8 C 0.05136(19) 0.05600(18) 0.59188(15) 0.0308(6) Uani 1 1 d . . .
C9 C 0.0762(2) -0.02901(19) 0.60081(17) 0.0377(7) Uani 1 1 d . . .
H9 H 0.0389 -0.0665 0.6292 0.045 Uiso 1 1 calc R U .
C10 C 0.1531(2) -0.0605(2) 0.56981(19) 0.0419(7) Uani 1 1 d . . .
C11 C 0.2057(2) -0.0056(2) 0.52695(18) 0.0385(7) Uani 1 1 d . . .
H11 H 0.2575 -0.0271 0.5034 0.046 Uiso 1 1 calc R U .
C12 C 0.18497(19) 0.07999(18) 0.51735(16) 0.0317(6) Uani 1 1 d . . .
C13 C -0.03692(19) 0.08248(19) 0.62071(17) 0.0358(7) Uani 1 1 d . . .
H13A H -0.0583 0.1300 0.5885 0.054 Uiso 1 1 calc R U .
H13B H -0.0329 0.1004 0.6762 0.054 Uiso 1 1 calc R U .
H13C H -0.0773 0.0344 0.6163 0.054 Uiso 1 1 calc R U .
C14 C 0.1788(3) -0.1528(2) 0.5809(3) 0.0629(11) Uani 1 1 d . . .
H14A H 0.1712 -0.1835 0.5308 0.094 Uiso 1 1 calc R U .
H14B H 0.1420 -0.1786 0.6217 0.094 Uiso 1 1 calc R U .
H14C H 0.2400 -0.1559 0.5973 0.094 Uiso 1 1 calc R U .
C15 C 0.2472(2) 0.13444(19) 0.47023(16) 0.0357(6) Uani 1 1 d . . .
H15A H 0.2902 0.0980 0.4439 0.054 Uiso 1 1 calc R U .
H15B H 0.2772 0.1741 0.5058 0.054 Uiso 1 1 calc R U .
H15C H 0.2146 0.1667 0.4303 0.054 Uiso 1 1 calc R U .
C16 C -0.01466(18) 0.40430(17) 0.63381(15) 0.0279(6) Uani 1 1 d . . .
C17 C -0.10557(18) 0.40824(19) 0.64753(17) 0.0331(6) Uani 1 1 d . . .
C18 C -0.1395(2) 0.4789(2) 0.68585(17) 0.0374(7) Uani 1 1 d . . .
H18 H -0.2007 0.4821 0.6940 0.045 Uiso 1 1 calc R U .
C19 C -0.0876(2) 0.54486(19) 0.71270(16) 0.0349(6) Uani 1 1 d . . .
C20 C 0.0015(2) 0.53735(18) 0.70266(16) 0.0334(6) Uani 1 1 d . . .
H20 H 0.0384 0.5807 0.7230 0.040 Uiso 1 1 calc R U .
C21 C 0.03887(18) 0.46820(18) 0.66373(16) 0.0310(6) Uani 1 1 d . . .
C22 C -0.1650(2) 0.3373(2) 0.6220(2) 0.0481(8) Uani 1 1 d . . .
H22A H -0.1636 0.3323 0.5641 0.072 Uiso 1 1 calc R U .
H22B H -0.2246 0.3497 0.6393 0.072 Uiso 1 1 calc R U .
H22C H -0.1454 0.2837 0.6458 0.072 Uiso 1 1 calc R U .
C23 C -0.1264(2) 0.6227(2) 0.7517(2) 0.0492(8) Uani 1 1 d . . .
H23A H -0.1643 0.6523 0.7139 0.074 Uiso 1 1 calc R U .
H23B H -0.0795 0.6610 0.7686 0.074 Uiso 1 1 calc R U .
H23C H -0.1607 0.6054 0.7980 0.074 Uiso 1 1 calc R U .
C24 C 0.1362(2) 0.4648(2) 0.6562(2) 0.0485(8) Uani 1 1 d . . .
H24A H 0.1519 0.4338 0.6079 0.073 Uiso 1 1 calc R U .
H24B H 0.1608 0.4355 0.7023 0.073 Uiso 1 1 calc R U .
H24C H 0.1595 0.5228 0.6535 0.073 Uiso 1 1 calc R U .
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 '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
N1 Sb1 N1 177.81(9) 2 .
N1 Sb1 Sb1 88.91(4) 2 3_556
N1 Sb1 Sb1 88.91(4) . 3_556
N1 P1 N1 104.61(14) . 4_556
C1 N1 P1 120.33(16) . .
C1 N1 Sb1 110.12(14) . .
P1 N1 Sb1 128.78(10) . .
C6 C1 C2 119.4(2) . .
C6 C1 N1 121.0(2) . .
C2 C1 N1 119.5(2) . .
C3 C2 C1 118.8(2) . .
C3 C2 C7 116.2(2) . .
C1 C2 C7 124.7(2) . .
C4 C3 C2 121.7(3) . .
C4 C3 H3 119.2 . .
C2 C3 H3 119.2 . .
C5 C4 C3 119.4(3) . .
C5 C4 H4 120.3 . .
C3 C4 H4 120.3 . .
C4 C5 C6 121.3(3) . .
C4 C5 H5 119.4 . .
C6 C5 H5 119.4 . .
C5 C6 C1 119.2(3) . .
C5 C6 C16 114.5(2) . .
C1 C6 C16 126.2(2) . .
C8 C7 C12 119.4(3) . .
C8 C7 C2 118.4(2) . .
C12 C7 C2 121.6(2) . .
C9 C8 C7 118.8(3) . .
C9 C8 C13 118.5(3) . .
C7 C8 C13 122.6(3) . .
C10 C9 C8 122.3(3) . .
C10 C9 H9 118.8 . .
C8 C9 H9 118.8 . .
C9 C10 C11 118.2(3) . .
C9 C10 C14 121.3(3) . .
C11 C10 C14 120.6(3) . .
C10 C11 C12 122.0(3) . .
C10 C11 H11 119.0 . .
C12 C11 H11 119.0 . .
C11 C12 C7 119.2(3) . .
C11 C12 C15 117.7(3) . .
C7 C12 C15 123.1(3) . .
C8 C13 H13A 109.5 . .
C8 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
C8 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
C10 C14 H14A 109.5 . .
C10 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C10 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
C12 C15 H15A 109.5 . .
C12 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
C12 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
C21 C16 C17 119.4(3) . .
C21 C16 C6 122.2(2) . .
C17 C16 C6 117.7(2) . .
C18 C17 C16 118.8(3) . .
C18 C17 C22 120.0(3) . .
C16 C17 C22 121.2(3) . .
C19 C18 C17 122.5(3) . .
C19 C18 H18 118.8 . .
C17 C18 H18 118.8 . .
C20 C19 C18 117.7(3) . .
C20 C19 C23 120.8(3) . .
C18 C19 C23 121.5(3) . .
C19 C20 C21 122.1(3) . .
C19 C20 H20 118.9 . .
C21 C20 H20 118.9 . .
C16 C21 C20 119.4(3) . .
C16 C21 C24 122.1(3) . .
C20 C21 C24 118.5(3) . .
C17 C22 H22A 109.5 . .
C17 C22 H22B 109.5 . .
H22A C22 H22B 109.5 . .
C17 C22 H22C 109.5 . .
H22A C22 H22C 109.5 . .
H22B C22 H22C 109.5 . .
C19 C23 H23A 109.5 . .
C19 C23 H23B 109.5 . .
H23A C23 H23B 109.5 . .
C19 C23 H23C 109.5 . .
H23A C23 H23C 109.5 . .
H23B C23 H23C 109.5 . .
C21 C24 H24A 109.5 . .
C21 C24 H24B 109.5 . .
H24A C24 H24B 109.5 . .
C21 C24 H24C 109.5 . .
H24A C24 H24C 109.5 . .
H24B C24 H24C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sb1 N1 2.372(2) 2
Sb1 N1 2.372(2) .
Sb1 Sb1 2.6438(4) 3_556
P1 N1 1.613(2) .
P1 N1 1.613(2) 4_556
N1 C1 1.432(3) .
C1 C6 1.407(4) .
C1 C2 1.415(4) .
C2 C3 1.392(4) .
C2 C7 1.496(4) .
C3 C4 1.379(4) .
C3 H3 0.9500 .
C4 C5 1.376(4) .
C4 H4 0.9500 .
C5 C6 1.399(4) .
C5 H5 0.9500 .
C6 C16 1.503(4) .
C7 C8 1.407(4) .
C7 C12 1.413(4) .
C8 C9 1.397(4) .
C8 C13 1.498(4) .
C9 C10 1.383(4) .
C9 H9 0.9500 .
C10 C11 1.385(4) .
C10 C14 1.513(5) .
C11 C12 1.392(4) .
C11 H11 0.9500 .
C12 C15 1.508(4) .
C13 H13A 0.9800 .
C13 H13B 0.9800 .
C13 H13C 0.9800 .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
C15 H15A 0.9800 .
C15 H15B 0.9800 .
C15 H15C 0.9800 .
C16 C21 1.392(4) .
C16 C17 1.415(4) .
C17 C18 1.386(4) .
C17 C22 1.502(4) .
C18 C19 1.383(4) .
C18 H18 0.9500 .
C19 C20 1.382(4) .
C19 C23 1.512(4) .
C20 C21 1.393(4) .
C20 H20 0.9500 .
C21 C24 1.499(4) .
C22 H22A 0.9800 .
C22 H22B 0.9800 .
C22 H22C 0.9800 .
C23 H23A 0.9800 .
C23 H23B 0.9800 .
C23 H23C 0.9800 .
C24 H24A 0.9800 .
C24 H24B 0.9800 .
C24 H24C 0.9800 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
N1 P1 N1 C1 -169.4(2) 4_556
N1 P1 N1 Sb1 -0.51(7) 4_556
P1 N1 C1 C6 60.0(3) .
Sb1 N1 C1 C6 -110.8(2) .
P1 N1 C1 C2 -124.5(2) .
Sb1 N1 C1 C2 64.6(3) .
C6 C1 C2 C3 4.9(4) .
N1 C1 C2 C3 -170.6(2) .
C6 C1 C2 C7 -168.4(3) .
N1 C1 C2 C7 16.1(4) .
C1 C2 C3 C4 -0.9(4) .
C7 C2 C3 C4 173.0(3) .
C2 C3 C4 C5 -2.5(5) .
C3 C4 C5 C6 1.8(5) .
C4 C5 C6 C1 2.3(4) .
C4 C5 C6 C16 -174.7(3) .
C2 C1 C6 C5 -5.6(4) .
N1 C1 C6 C5 169.8(2) .
C2 C1 C6 C16 171.0(3) .
N1 C1 C6 C16 -13.5(4) .
C3 C2 C7 C8 -107.2(3) .
C1 C2 C7 C8 66.3(3) .
C3 C2 C7 C12 63.4(3) .
C1 C2 C7 C12 -123.1(3) .
C12 C7 C8 C9 4.2(4) .
C2 C7 C8 C9 175.0(2) .
C12 C7 C8 C13 -171.8(2) .
C2 C7 C8 C13 -0.9(4) .
C7 C8 C9 C10 -1.9(4) .
C13 C8 C9 C10 174.2(3) .
C8 C9 C10 C11 -1.5(4) .
C8 C9 C10 C14 179.5(3) .
C9 C10 C11 C12 2.7(5) .
C14 C10 C11 C12 -178.4(3) .
C10 C11 C12 C7 -0.3(4) .
C10 C11 C12 C15 179.4(3) .
C8 C7 C12 C11 -3.1(4) .
C2 C7 C12 C11 -173.6(2) .
C8 C7 C12 C15 177.1(2) .
C2 C7 C12 C15 6.6(4) .
C5 C6 C16 C21 -98.9(3) .
C1 C6 C16 C21 84.3(4) .
C5 C6 C16 C17 71.4(3) .
C1 C6 C16 C17 -105.4(3) .
C21 C16 C17 C18 4.4(4) .
C6 C16 C17 C18 -166.2(2) .
C21 C16 C17 C22 -175.1(3) .
C6 C16 C17 C22 14.3(4) .
C16 C17 C18 C19 -1.4(4) .
C22 C17 C18 C19 178.1(3) .
C17 C18 C19 C20 -2.2(4) .
C17 C18 C19 C23 177.8(3) .
C18 C19 C20 C21 3.0(4) .
C23 C19 C20 C21 -177.0(3) .
C17 C16 C21 C20 -3.7(4) .
C6 C16 C21 C20 166.5(2) .
C17 C16 C21 C24 175.7(3) .
C6 C16 C21 C24 -14.2(4) .
C19 C20 C21 C16 0.0(4) .
C19 C20 C21 C24 -179.4(3) .
