#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:08:04 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179314 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/11/4321128.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_4321128
loop_
_publ_author_name
'Ingo Schranz'
'Luke P. Grocholl'
'Lothar Stahl'
'Richard J. Staples'
'Alison Johnson'
_publ_section_title
;
 Syntheses and Structures of Heterobicyclic
 Bis(tert-butylamido)cyclodiphosph(III)azane Compounds Having
 Phosphorus(III) and Arsenic(III) Centers
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3037
_journal_page_last               3041
_journal_paper_doi               10.1021/ic991405r
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C16 H34 N7 P3'
_chemical_formula_weight         417.41
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 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                 97.23(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.496(7)
_cell_length_b                   12.455(7)
_cell_length_c                   10.043(6)
_cell_measurement_reflns_used    31
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      19.30
_cell_measurement_theta_min      3.92
_cell_volume                     1178.4(13)
_computing_cell_refinement       'SMART (SIEMENS, V4.033, 1994)'
_computing_data_collection       'ASTRO (SIEMENS, V4.033, 1994)'
_computing_data_reduction        'SAINT (SIEMENS, V4.035, 1994)'
_computing_molecular_graphics    'SHELXTL (SIEMENS, 1994, ver 5.04)'
_computing_publication_material  'CIFTAB (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_method       'ω, 0.3 deg'
_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  0.0433
_diffrn_reflns_av_sigmaI/netI    0.0531
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            6087
_diffrn_reflns_theta_full        24.72
_diffrn_reflns_theta_max         24.72
_diffrn_reflns_theta_min         2.04
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.267
_exptl_absorpt_correction_T_max  0.942272
_exptl_absorpt_correction_T_min  0.820494
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.176
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chunk
_exptl_crystal_F_000             448
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.251
_refine_diff_density_min         -0.368
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     133
_refine_ls_number_reflns         2111
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0810
_refine_ls_R_factor_gt           0.0499
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0455P)²+0.8768P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1073
_refine_ls_wR_factor_ref         0.1216
_reflns_number_gt                1527
_reflns_number_total             2111
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic991405r_1.cif
_cod_data_source_block           Compound2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4321128
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
P2 P 0.36737(11) 0.2500 0.26887(11) 0.0352(3) Uani 1 2 d S . .
P1 P 0.10005(8) 0.14837(7) 0.12647(8) 0.0373(3) Uani 1 1 d . . .
N2 N 0.0431(3) 0.2500 0.2215(3) 0.0366(9) Uani 1 2 d S . .
N1 N 0.1078(3) 0.2500 0.0120(3) 0.0370(9) Uani 1 2 d S . .
N3 N 0.2759(2) 0.14248(19) 0.2000(2) 0.0341(6) Uani 1 1 d . . .
N4 N 0.3098(4) 0.2500 0.4383(4) 0.0495(10) Uani 1 2 d S . .
N5 N 0.4098(4) 0.2500 0.5271(4) 0.0441(9) Uani 1 2 d S . .
N6 N 0.5007(5) 0.2500 0.6134(4) 0.0644(13) Uani 1 2 d S . .
C1 C 0.1742(5) 0.2500 -0.1147(4) 0.0481(12) Uani 1 2 d S . .
C2 C 0.1241(5) 0.1494(4) -0.1924(4) 0.0798(13) Uani 1 1 d . . .
H2A H 0.1572 0.0864 -0.1410 0.120 Uiso 1 1 calc R . .
H2B H 0.1619 0.1488 -0.2778 0.120 Uiso 1 1 calc R . .
H2C H 0.0212 0.1488 -0.2081 0.120 Uiso 1 1 calc R . .
C3 C 0.3377(5) 0.2500 -0.0892(5) 0.0615(15) Uani 1 2 d S . .
H3A H 0.3703 0.1866 -0.0402 0.092 Uiso 0.50 1 d PR . .
H3B H 0.3746 0.2500 -0.1739 0.092 Uiso 1 2 d SR . .
C4 C -0.0873(4) 0.2500 0.2898(5) 0.0442(12) Uani 1 2 d S . .
C5 C -0.0840(4) 0.1503(3) 0.3755(4) 0.0737(12) Uani 1 1 d . . .
H5A H -0.0862 0.0872 0.3187 0.110 Uiso 1 1 calc R . .
H5B H -0.1659 0.1498 0.4243 0.110 Uiso 1 1 calc R . .
H5C H 0.0021 0.1498 0.4387 0.110 Uiso 1 1 calc R . .
C6 C -0.2189(5) 0.2500 0.1831(6) 0.0697(17) Uani 1 2 d S . .
H6A H -0.2190 0.3135 0.1289 0.105 Uiso 0.50 1 d PR . .
H6B H -0.3028 0.2500 0.2274 0.105 Uiso 1 2 d SR . .
C7 C 0.3370(3) 0.0320(2) 0.2354(3) 0.0405(8) Uani 1 1 d . . .
C8 C 0.3110(4) -0.0405(3) 0.1123(3) 0.0566(10) Uani 1 1 d . . .
H8A H 0.2098 -0.0449 0.0830 0.085 Uiso 1 1 calc R . .
H8B H 0.3477 -0.1117 0.1351 0.085 Uiso 1 1 calc R . .
H8C H 0.3587 -0.0110 0.0407 0.085 Uiso 1 1 calc R . .
C9 C 0.2633(4) -0.0156(3) 0.3490(3) 0.0541(9) Uani 1 1 d . . .
H9A H 0.2797 0.0304 0.4273 0.081 Uiso 1 1 calc R . .
H9B H 0.3014 -0.0866 0.3713 0.081 Uiso 1 1 calc R . .
H9C H 0.1621 -0.0209 0.3203 0.081 Uiso 1 1 calc R . .
C10 C 0.4968(3) 0.0375(3) 0.2793(4) 0.0553(9) Uani 1 1 d . . .
H10A H 0.5154 0.0834 0.3576 0.083 Uiso 1 1 calc R . .
H10B H 0.5437 0.0666 0.2069 0.083 Uiso 1 1 calc R . .
H10C H 0.5328 -0.0341 0.3014 0.083 Uiso 1 1 calc R . .
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'
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
_geom_angle_publ_flag
P2 P2 N3 0(10) 4_565 . ?
P2 P2 N3 0(10) 4_565 4_565 ?
N3 P2 N3 104.30(17) . 4_565 ?
P2 P2 N4 0(10) 4_565 . ?
N3 P2 N4 100.35(11) . . ?
N3 P2 N4 100.35(11) 4_565 . ?
N2 P1 N1 82.61(13) . . ?
N2 P1 N3 98.53(14) . . ?
N1 P1 N3 101.28(14) . . ?
N2 P1 P1 42.36(9) . 4_565 ?
N1 P1 P1 42.53(9) . 4_565 ?
N3 P1 P1 92.42(8) . 4_565 ?
C4 N2 P1 126.57(14) . . ?
C4 N2 P1 126.57(14) . 4_565 ?
P1 N2 P1 95.27(17) . 4_565 ?
C1 N1 P1 129.05(12) . 4_565 ?
C1 N1 P1 129.05(12) . . ?
P1 N1 P1 94.93(18) 4_565 . ?
C7 N3 P2 117.30(19) . 4_565 ?
C7 N3 P2 117.30(19) . . ?
P2 N3 P2 0.00(7) 4_565 . ?
C7 N3 P1 117.13(19) . . ?
P2 N3 P1 123.71(15) 4_565 . ?
P2 N3 P1 123.71(15) . . ?
N5 N4 P2 112.3(3) . 4_565 ?
N5 N4 P2 112.3(3) . . ?
P2 N4 P2 0.00(2) 4_565 . ?
N6 N5 N4 177.8(5) . . ?
N1 C1 C2 107.4(3) . . ?
N1 C1 C2 107.4(3) . 4_565 ?
C2 C1 C2 111.0(4) . 4_565 ?
N1 C1 C3 112.6(4) . . ?
C2 C1 C3 109.2(3) . . ?
C2 C1 C3 109.2(3) 4_565 . ?
N2 C4 C5 107.7(2) . 4_565 ?
N2 C4 C5 107.7(2) . . ?
C5 C4 C5 110.8(4) 4_565 . ?
N2 C4 C6 109.1(4) . . ?
C5 C4 C6 110.7(3) 4_565 . ?
C5 C4 C6 110.7(3) . . ?
N3 C7 C8 109.2(2) . . ?
N3 C7 C10 111.4(2) . . ?
C8 C7 C10 108.3(3) . . ?
N3 C7 C9 109.2(2) . . ?
C8 C7 C9 109.3(3) . . ?
C10 C7 C9 109.4(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P2 P2 0.000(2) 4_565 ?
P2 N3 1.696(3) . ?
P2 N3 1.696(3) 4_565 ?
P2 N4 1.852(4) . ?
P1 N2 1.713(2) . ?
P1 N1 1.718(2) . ?
P1 N3 1.740(3) . ?
P1 P1 2.532(2) 4_565 ?
N2 C4 1.489(5) . ?
N2 P1 1.713(2) 4_565 ?
N1 C1 1.489(5) . ?
N1 P1 1.718(2) 4_565 ?
N3 C7 1.518(4) . ?
N3 P2 1.696(3) 4_565 ?
N4 N5 1.218(5) . ?
N4 P2 1.852(4) 4_565 ?
N5 N6 1.144(5) . ?
C1 C2 1.521(4) . ?
C1 C2 1.521(4) 4_565 ?
C1 C3 1.542(7) . ?
C4 C5 1.509(4) 4_565 ?
C4 C5 1.509(4) . ?
C4 C6 1.541(7) . ?
C7 C8 1.526(4) . ?
C7 C10 1.528(4) . ?
C7 C9 1.531(4) . ?
