#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:30:40 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179114 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/76/4307674.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_4307674
loop_
_publ_author_name
'Shaun P. Green'
'Cameron Jones'
'Guoxia Jin'
'Andreas Stasch'
_publ_section_title
;
Base-Stabilized Amidodiarsenes: Synthesis, Structure, and Theoretical
Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8
_journal_page_last               10
_journal_paper_doi               10.1021/ic062163f
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C37 H56 Cl2 N3 P'
_chemical_formula_weight         644.72
_chemical_name_systematic
; 
 ? 
;
_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                 98.55(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.3103(19)
_cell_length_b                   18.450(4)
_cell_length_c                   20.787(4)
_cell_measurement_temperature    150(2)
_cell_volume                     3531.0(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_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  0.0390
_diffrn_reflns_av_sigmaI/netI    0.0606
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            13106
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.96
_exptl_absorpt_coefficient_mu    0.259
_exptl_absorpt_correction_T_max  0.938
_exptl_absorpt_correction_T_min  0.880
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav (Blessing, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.798
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     396
_refine_ls_number_reflns         6930
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0820
_refine_ls_R_factor_gt           0.0560
_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)+(0.0759P)²+2.2110P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1430
_refine_ls_wR_factor_ref         0.1583
_reflns_number_gt                5100
_reflns_number_total             6930
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic062163fsi20061114_083022.cif
_cod_data_source_block           compound1
_cod_original_cell_volume        3530.9(12)
_cod_database_code               4307674
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl1 Cl 0.80562(10) 0.70592(4) 0.26137(4) 0.0439(2) Uani 1 1 d . . .
P1 P 0.78529(8) 0.81651(4) 0.23906(3) 0.02728(19) Uani 1 1 d . . .
N1 N 0.9378(2) 0.84400(10) 0.20295(9) 0.0212(5) Uani 1 1 d . . .
C1 C 1.0282(3) 0.85985(12) 0.26030(11) 0.0199(5) Uani 1 1 d . . .
Cl2 Cl 0.65466(8) 0.78785(4) 0.14013(3) 0.0391(2) Uani 1 1 d . . .
N2 N 0.9516(2) 0.83616(10) 0.30570(9) 0.0206(4) Uani 1 1 d . . .
C2 C 0.9683(3) 0.84184(13) 0.13679(11) 0.0215(5) Uani 1 1 d . . .
N3 N 1.1598(2) 0.89062(11) 0.26843(9) 0.0244(5) Uani 1 1 d . . .
C3 C 0.9110(3) 0.89678(13) 0.09366(11) 0.0240(6) Uani 1 1 d . . .
C4 C 0.9494(3) 0.89656(14) 0.03145(12) 0.0286(6) Uani 1 1 d . . .
H4 H 0.9138 0.9337 0.0016 0.034 Uiso 1 1 calc R . .
C5 C 1.0382(3) 0.84347(15) 0.01232(12) 0.0317(6) Uani 1 1 d . . .
H5 H 1.0656 0.8452 -0.0299 0.038 Uiso 1 1 calc R . .
C6 C 1.0875(3) 0.78782(14) 0.05419(13) 0.0301(6) Uani 1 1 d . . .
H6 H 1.1457 0.7506 0.0399 0.036 Uiso 1 1 calc R . .
C7 C 1.0531(3) 0.78547(13) 0.11737(12) 0.0249(6) Uani 1 1 d . . .
C8 C 0.8040(3) 0.95378(14) 0.11120(12) 0.0277(6) Uani 1 1 d . . .
H8 H 0.7588 0.9346 0.1485 0.033 Uiso 1 1 calc R . .
C9 C 0.8766(4) 1.02638(15) 0.13238(15) 0.0389(7) Uani 1 1 d . . .
H9A H 0.9455 1.0194 0.1724 0.058 Uiso 1 1 calc R . .
H9B H 0.8023 1.0615 0.1403 0.058 Uiso 1 1 calc R . .
H9C H 0.9286 1.0446 0.0980 0.058 Uiso 1 1 calc R . .
C10 C 0.6820(4) 0.96732(17) 0.05455(14) 0.0416(7) Uani 1 1 d . . .
H10A H 0.7224 0.9899 0.0185 0.062 Uiso 1 1 calc R . .
H10B H 0.6094 0.9996 0.0688 0.062 Uiso 1 1 calc R . .
H10C H 0.6363 0.9211 0.0401 0.062 Uiso 1 1 calc R . .
C11 C 1.1001(3) 0.72035(14) 0.16016(13) 0.0313(6) Uani 1 1 d . . .
H11 H 1.0873 0.7326 0.2058 0.038 Uiso 1 1 calc R . .
C12 C 0.9988(4) 0.65640(16) 0.13719(16) 0.0469(8) Uani 1 1 d . . .
H12A H 0.8975 0.6713 0.1364 0.070 Uiso 1 1 calc R . .
H12B H 1.0204 0.6155 0.1672 0.070 Uiso 1 1 calc R . .
H12C H 1.0141 0.6417 0.0934 0.070 Uiso 1 1 calc R . .
C13 C 1.2572(4) 0.69738(17) 0.16010(18) 0.0499(9) Uani 1 1 d . . .
H13A H 1.2701 0.6817 0.1163 0.075 Uiso 1 1 calc R . .
H13B H 1.2809 0.6572 0.1907 0.075 Uiso 1 1 calc R . .
H13C H 1.3217 0.7384 0.1733 0.075 Uiso 1 1 calc R . .
C14 C 0.9400(3) 0.86572(13) 0.36860(11) 0.0210(5) Uani 1 1 d . . .
C15 C 0.8918(3) 0.93749(13) 0.37468(12) 0.0253(6) Uani 1 1 d . . .
C16 C 0.8672(3) 0.96064(15) 0.43599(13) 0.0325(6) Uani 1 1 d . . .
H16 H 0.8333 1.0086 0.4412 0.039 Uiso 1 1 calc R . .
C17 C 0.8911(3) 0.91528(15) 0.48919(13) 0.0347(7) Uani 1 1 d . . .
H17 H 0.8743 0.9323 0.5306 0.042 Uiso 1 1 calc R . .
C18 C 0.9390(3) 0.84552(15) 0.48283(12) 0.0310(6) Uani 1 1 d . . .
H18 H 0.9561 0.8151 0.5201 0.037 Uiso 1 1 calc R . .
C19 C 0.9632(3) 0.81856(13) 0.42236(11) 0.0236(5) Uani 1 1 d . . .
C20 C 0.8615(3) 0.99017(14) 0.31730(12) 0.0277(6) Uani 1 1 d . . .
H20 H 0.9047 0.9692 0.2802 0.033 Uiso 1 1 calc R . .
C21 C 0.6983(3) 0.99912(16) 0.29536(15) 0.0404(7) Uani 1 1 d . . .
H21A H 0.6556 0.9520 0.2818 0.061 Uiso 1 1 calc R . .
H21B H 0.6820 1.0330 0.2587 0.061 Uiso 1 1 calc R . .
H21C H 0.6529 1.0181 0.3315 0.061 Uiso 1 1 calc R . .
C22 C 0.9306(3) 1.06496(15) 0.33290(14) 0.0366(7) Uani 1 1 d . . .
H22A H 0.8829 1.0888 0.3662 0.055 Uiso 1 1 calc R . .
H22B H 0.9186 1.0947 0.2934 0.055 Uiso 1 1 calc R . .
H22C H 1.0343 1.0591 0.3491 0.055 Uiso 1 1 calc R . .
C23 C 1.0083(3) 0.74019(14) 0.41734(12) 0.0275(6) Uani 1 1 d . . .
H23 H 1.0190 0.7303 0.3710 0.033 Uiso 1 1 calc R . .
C24 C 1.1524(4) 0.72321(17) 0.45929(15) 0.0416(7) Uani 1 1 d . . .
H24A H 1.2276 0.7557 0.4476 0.062 Uiso 1 1 calc R . .
H24B H 1.1795 0.6729 0.4521 0.062 Uiso 1 1 calc R . .
H24C H 1.1431 0.7301 0.5052 0.062 Uiso 1 1 calc R . .
C25 C 0.8907(4) 0.68980(15) 0.43579(16) 0.0403(7) Uani 1 1 d . . .
H25A H 0.8830 0.6960 0.4820 0.060 Uiso 1 1 calc R . .
H25B H 0.9162 0.6394 0.4278 0.060 Uiso 1 1 calc R . .
H25C H 0.7973 0.7016 0.4095 0.060 Uiso 1 1 calc R . .
C26 C 1.2066(3) 0.93626(13) 0.21531(12) 0.0262(6) Uani 1 1 d . . .
H26 H 1.1177 0.9436 0.1825 0.031 Uiso 1 1 calc R . .
C27 C 1.2571(4) 1.01203(15) 0.23873(13) 0.0353(7) Uani 1 1 d . . .
H27A H 1.3493 1.0083 0.2691 0.042 Uiso 1 1 calc R . .
H27B H 1.1835 1.0344 0.2623 0.042 Uiso 1 1 calc R . .
C28 C 1.2797(4) 1.05998(16) 0.18056(14) 0.0409(8) Uani 1 1 d . . .
H28A H 1.1848 1.0687 0.1532 0.049 Uiso 1 1 calc R . .
H28B H 1.3196 1.1074 0.1967 0.049 Uiso 1 1 calc R . .
C29 C 1.3821(3) 1.02527(16) 0.13966(14) 0.0389(7) Uani 1 1 d . . .
H29A H 1.4810 1.0234 0.1649 0.047 Uiso 1 1 calc R . .
H29B H 1.3864 1.0553 0.1005 0.047 Uiso 1 1 calc R . .
C30 C 1.3336(4) 0.94872(16) 0.11876(13) 0.0376(7) Uani 1 1 d . . .
H30A H 1.4051 0.9267 0.0938 0.045 Uiso 1 1 calc R . .
H30B H 1.2387 0.9509 0.0901 0.045 Uiso 1 1 calc R . .
C31 C 1.3197(3) 0.90164(15) 0.17846(12) 0.0312(6) Uani 1 1 d . . .
H31A H 1.2890 0.8520 0.1645 0.037 Uiso 1 1 calc R . .
H31B H 1.4146 0.8986 0.2070 0.037 Uiso 1 1 calc R . .
C32 C 1.2571(3) 0.87648(17) 0.33224(13) 0.0364(7) Uani 1 1 d . . .
H32 H 1.2094 0.8361 0.3533 0.044 Uiso 1 1 calc R . .
C33 C 1.2678(4) 0.93963(17) 0.38111(13) 0.0395(7) Uani 1 1 d . . .
H33A H 1.3162 0.9813 0.3634 0.047 Uiso 1 1 calc R . .
H33B H 1.1689 0.9550 0.3873 0.047 Uiso 1 1 calc R . .
C34 C 1.3537(4) 0.9174(2) 0.44699(17) 0.0631(11) Uani 1 1 d . . .
H34A H 1.3663 0.9601 0.4762 0.076 Uiso 1 1 calc R . .
H34B H 1.2986 0.8802 0.4674 0.076 Uiso 1 1 calc R . .
C35 C 1.4967(5) 0.8884(3) 0.43887(18) 0.0740(13) Uani 1 1 d . . .
H35A H 1.5462 0.8717 0.4818 0.089 Uiso 1 1 calc R . .
H35B H 1.5557 0.9282 0.4243 0.089 Uiso 1 1 calc R . .
C36 C 1.4929(4) 0.8264(2) 0.39094(18) 0.0655(12) Uani 1 1 d . . .
H36A H 1.4476 0.7834 0.4082 0.079 Uiso 1 1 calc R . .
H36B H 1.5931 0.8133 0.3849 0.079 Uiso 1 1 calc R . .
C37 C 1.4048(4) 0.8487(2) 0.32488(17) 0.0566(10) Uani 1 1 d . . .
H37A H 1.4585 0.8868 0.3048 0.068 Uiso 1 1 calc R . .
H37B H 1.3946 0.8063 0.2954 0.068 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'
Cl Cl 0.1484 0.1585 '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
N1 P1 N2 69.33(9) . . ?
N1 P1 Cl1 108.67(8) . . ?
N2 P1 Cl1 89.30(7) . . ?
N1 P1 Cl2 92.17(7) . . ?
N2 P1 Cl2 159.98(7) . . ?
Cl1 P1 Cl2 89.56(4) . . ?
C1 N1 C2 130.2(2) . . ?
C1 N1 P1 96.80(14) . . ?
C2 N1 P1 132.56(17) . . ?
N3 C1 N2 128.6(2) . . ?
N3 C1 N1 128.8(2) . . ?
N2 C1 N1 102.6(2) . . ?
C1 N2 C14 129.7(2) . . ?
C1 N2 P1 90.57(15) . . ?
C14 N2 P1 123.88(16) . . ?
C7 C2 C3 121.9(2) . . ?
C7 C2 N1 119.5(2) . . ?
C3 C2 N1 118.5(2) . . ?
C1 N3 C26 120.3(2) . . ?
C1 N3 C32 117.1(2) . . ?
C26 N3 C32 122.6(2) . . ?
C4 C3 C2 117.7(2) . . ?
C4 C3 C8 119.3(2) . . ?
C2 C3 C8 122.9(2) . . ?
C5 C4 C3 121.2(2) . . ?
C4 C5 C6 120.3(2) . . ?
C5 C6 C7 121.0(3) . . ?
C6 C7 C2 117.7(2) . . ?
C6 C7 C11 119.2(2) . . ?
C2 C7 C11 122.9(2) . . ?
C3 C8 C10 111.3(2) . . ?
C3 C8 C9 113.2(2) . . ?
C10 C8 C9 108.9(2) . . ?
C7 C11 C13 114.3(2) . . ?
C7 C11 C12 108.3(2) . . ?
C13 C11 C12 109.3(2) . . ?
C19 C14 C15 121.5(2) . . ?
C19 C14 N2 117.7(2) . . ?
C15 C14 N2 120.4(2) . . ?
C16 C15 C14 117.8(2) . . ?
C16 C15 C20 118.7(2) . . ?
C14 C15 C20 123.4(2) . . ?
C17 C16 C15 121.2(3) . . ?
C18 C17 C16 120.5(2) . . ?
C17 C18 C19 121.1(2) . . ?
C18 C19 C14 117.8(2) . . ?
C18 C19 C23 119.0(2) . . ?
C14 C19 C23 123.2(2) . . ?
C21 C20 C15 111.1(2) . . ?
C21 C20 C22 109.4(2) . . ?
C15 C20 C22 112.5(2) . . ?
C19 C23 C24 112.8(2) . . ?
C19 C23 C25 110.3(2) . . ?
C24 C23 C25 109.6(2) . . ?
N3 C26 C31 115.4(2) . . ?
N3 C26 C27 112.8(2) . . ?
C31 C26 C27 109.8(2) . . ?
C26 C27 C28 110.3(2) . . ?
C29 C28 C27 111.7(3) . . ?
C28 C29 C30 111.5(2) . . ?
C29 C30 C31 110.5(2) . . ?
C26 C31 C30 108.4(2) . . ?
C37 C32 N3 114.1(2) . . ?
C37 C32 C33 110.9(3) . . ?
N3 C32 C33 114.8(2) . . ?
C34 C33 C32 111.1(3) . . ?
C35 C34 C33 110.8(3) . . ?
C34 C35 C36 114.7(4) . . ?
C35 C36 C37 109.9(3) . . ?
C32 C37 C36 112.0(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
Cl1 P1 2.0947(11) . ?
P1 N1 1.776(2) . ?
P1 N2 1.952(2) . ?
P1 Cl2 2.2899(12) . ?
N1 C1 1.385(3) . ?
N1 C2 1.445(3) . ?
C1 N3 1.338(3) . ?
C1 N2 1.338(3) . ?
N2 C14 1.436(3) . ?
C2 C7 1.401(4) . ?
C2 C3 1.405(3) . ?
N3 C26 1.503(3) . ?
N3 C32 1.513(3) . ?
C3 C4 1.392(3) . ?
C3 C8 1.529(4) . ?
C4 C5 1.378(4) . ?
C5 C6 1.380(4) . ?
C6 C7 1.398(3) . ?
C7 C11 1.520(4) . ?
C8 C10 1.530(4) . ?
C8 C9 1.535(4) . ?
C11 C13 1.523(4) . ?
C11 C12 1.541(4) . ?
C14 C19 1.407(3) . ?
C14 C15 1.410(4) . ?
C15 C16 1.395(4) . ?
C15 C20 1.532(3) . ?
C16 C17 1.378(4) . ?
C17 C18 1.375(4) . ?
C18 C19 1.401(3) . ?
C19 C23 1.513(4) . ?
C20 C21 1.529(4) . ?
C20 C22 1.536(4) . ?
C23 C24 1.521(4) . ?
C23 C25 1.528(4) . ?
C26 C31 1.531(4) . ?
C26 C27 1.531(4) . ?
C27 C28 1.538(4) . ?
C28 C29 1.511(4) . ?
C29 C30 1.526(4) . ?
C30 C31 1.536(4) . ?
C32 C37 1.496(5) . ?
C32 C33 1.539(4) . ?
C33 C34 1.535(4) . ?
C34 C35 1.468(6) . ?
C35 C36 1.515(6) . ?
C36 C37 1.547(5) . ?
