#------------------------------------------------------------------------------
#$Date: 2017-10-14 22:27:35 +0300 (Sat, 14 Oct 2017) $
#$Revision: 202017 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/15/7051581.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_7051581
loop_
_publ_author_name
'Jin, Guoxia'
'Jones, Cameron'
'Junk, Peter C.'
'Lippert, Kai-Alexander'
'Rose, Richard P.'
'Stasch, Andreas'
_publ_section_title
;
 Synthesis and characterisation of bulky guanidines and
 phosphaguanidines: precursors for low oxidation state metallacycles
;
_journal_issue                   1
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              64
_journal_paper_doi               10.1039/b809120j
_journal_volume                  33
_journal_year                    2009
_chemical_formula_sum            'C31 H49 N3'
_chemical_formula_weight         463.73
_chemical_name_systematic
;
?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.397(4)
_cell_length_b                   15.542(3)
_cell_length_c                   20.168(4)
_cell_measurement_temperature    150(2)
_cell_volume                     5767(2)
_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  0.0382
_diffrn_reflns_av_sigmaI/netI    0.0292
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            19664
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    0.062
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_correction_T_min  0.961
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav (Blessing, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.068
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.341
_refine_diff_density_min         -0.350
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         5343
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0435
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0495P)²+1.7216P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1004
_refine_ls_wR_factor_ref         0.1069
_reflns_number_gt                4348
_reflns_number_total             5343
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b809120j.txt
_cod_data_source_block           compound2
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               7051581
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.19631(6) 0.81979(6) 0.12567(5) 0.0216(2) Uani 1 1 d . . .
H1 H 0.2352 0.8484 0.1381 0.026 Uiso 1 1 calc R . .
C1 C 0.20960(6) 0.73754(8) 0.10134(6) 0.0192(3) Uani 1 1 d . . .
N2 N 0.26976(6) 0.71782(6) 0.07208(5) 0.0217(2) Uani 1 1 d . . .
C2 C 0.12879(7) 0.86523(8) 0.13361(6) 0.0217(3) Uani 1 1 d . . .
N3 N 0.15581(6) 0.67659(6) 0.10987(5) 0.0218(2) Uani 1 1 d . . .
C3 C 0.11273(7) 0.89852(8) 0.19682(7) 0.0243(3) Uani 1 1 d . . .
C4 C 0.04973(8) 0.94750(9) 0.20419(7) 0.0302(3) Uani 1 1 d . . .
H4 H 0.0385 0.9717 0.2462 0.036 Uiso 1 1 calc R . .
C5 C 0.00344(8) 0.96143(9) 0.15150(7) 0.0347(3) Uani 1 1 d . . .
H5 H -0.0395 0.9946 0.1574 0.042 Uiso 1 1 calc R . .
C6 C 0.01956(8) 0.92715(9) 0.09014(7) 0.0321(3) Uani 1 1 d . . .
H6 H -0.0131 0.9365 0.0544 0.039 Uiso 1 1 calc R . .
C7 C 0.08243(7) 0.87926(8) 0.07920(7) 0.0252(3) Uani 1 1 d . . .
C8 C 0.16164(7) 0.88238(9) 0.25661(7) 0.0280(3) Uani 1 1 d . . .
H8 H 0.1991 0.8393 0.2430 0.034 Uiso 1 1 calc R . .
C9 C 0.20143(11) 0.96344(12) 0.27712(9) 0.0586(5) Uani 1 1 d . . .
H9A H 0.2326 0.9828 0.2406 0.088 Uiso 1 1 calc R . .
H9B H 0.2314 0.9514 0.3162 0.088 Uiso 1 1 calc R . .
H9C H 0.1660 1.0085 0.2878 0.088 Uiso 1 1 calc R . .
C10 C 0.12056(10) 0.84486(13) 0.31539(8) 0.0511(5) Uani 1 1 d . . .
H10A H 0.0881 0.8887 0.3339 0.077 Uiso 1 1 calc R . .
H10B H 0.1553 0.8265 0.3494 0.077 Uiso 1 1 calc R . .
H10C H 0.0919 0.7953 0.3007 0.077 Uiso 1 1 calc R . .
C11 C 0.10051(8) 0.84805(9) 0.00973(7) 0.0280(3) Uani 1 1 d . . .
H11 H 0.1332 0.7970 0.0141 0.034 Uiso 1 1 calc R . .
C12 C 0.14217(8) 0.91753(10) -0.02815(8) 0.0356(3) Uani 1 1 d . . .
H12A H 0.1135 0.9707 -0.0288 0.053 Uiso 1 1 calc R . .
H12B H 0.1509 0.8982 -0.0737 0.053 Uiso 1 1 calc R . .
H12C H 0.1888 0.9283 -0.0062 0.053 Uiso 1 1 calc R . .
C13 C 0.03382(9) 0.82012(10) -0.03000(8) 0.0401(4) Uani 1 1 d . . .
H13A H 0.0038 0.8706 -0.0400 0.060 Uiso 1 1 calc R . .
H13B H 0.0054 0.7788 -0.0040 0.060 Uiso 1 1 calc R . .
H13C H 0.0495 0.7931 -0.0715 0.060 Uiso 1 1 calc R . .
C14 C 0.32443(7) 0.78054(8) 0.06253(6) 0.0216(3) Uani 1 1 d . . .
C15 C 0.36866(7) 0.80618(8) 0.11635(6) 0.0232(3) Uani 1 1 d . . .
C16 C 0.42391(7) 0.86580(8) 0.10480(7) 0.0281(3) Uani 1 1 d . . .
H16 H 0.4532 0.8845 0.1408 0.034 Uiso 1 1 calc R . .
C17 C 0.43691(7) 0.89817(9) 0.04217(7) 0.0310(3) Uani 1 1 d . . .
H17 H 0.4744 0.9393 0.0354 0.037 Uiso 1 1 calc R . .
C18 C 0.39529(7) 0.87066(9) -0.01052(7) 0.0293(3) Uani 1 1 d . . .
H18 H 0.4050 0.8926 -0.0536 0.035 Uiso 1 1 calc R . .
C19 C 0.33920(7) 0.81131(8) -0.00203(6) 0.0247(3) Uani 1 1 d . . .
C20 C 0.35980(7) 0.76430(9) 0.18392(6) 0.0263(3) Uani 1 1 d . . .
H20 H 0.3067 0.7547 0.1913 0.032 Uiso 1 1 calc R . .
C21 C 0.38800(9) 0.81883(11) 0.24107(7) 0.0423(4) Uani 1 1 d . . .
H21A H 0.4409 0.8246 0.2375 0.063 Uiso 1 1 calc R . .
H21B H 0.3757 0.7911 0.2832 0.063 Uiso 1 1 calc R . .
H21C H 0.3656 0.8760 0.2393 0.063 Uiso 1 1 calc R . .
C22 C 0.39691(9) 0.67609(10) 0.18378(8) 0.0376(4) Uani 1 1 d . . .
H22A H 0.3771 0.6410 0.1477 0.056 Uiso 1 1 calc R . .
H22B H 0.3881 0.6473 0.2262 0.056 Uiso 1 1 calc R . .
H22C H 0.4493 0.6835 0.1773 0.056 Uiso 1 1 calc R . .
C23 C 0.29789(8) 0.77413(9) -0.06036(7) 0.0298(3) Uani 1 1 d . . .
H23 H 0.2461 0.7667 -0.0465 0.036 Uiso 1 1 calc R . .
C24 C 0.32853(9) 0.68462(9) -0.07626(7) 0.0355(3) Uani 1 1 d . . .
H24A H 0.3792 0.6900 -0.0906 0.053 Uiso 1 1 calc R . .
H24B H 0.2998 0.6583 -0.1118 0.053 Uiso 1 1 calc R . .
H24C H 0.3262 0.6484 -0.0365 0.053 Uiso 1 1 calc R . .
C25 C 0.29871(9) 0.83083(11) -0.12258(7) 0.0411(4) Uani 1 1 d . . .
H25A H 0.2825 0.8890 -0.1111 0.062 Uiso 1 1 calc R . .
H25B H 0.2660 0.8064 -0.1560 0.062 Uiso 1 1 calc R . .
H25C H 0.3482 0.8334 -0.1405 0.062 Uiso 1 1 calc R . .
C26 C 0.10875(7) 0.67707(8) 0.16906(7) 0.0256(3) Uani 1 1 d . . .
H26 H 0.1150 0.7345 0.1906 0.031 Uiso 1 1 calc R . .
C27 C 0.02859(8) 0.66928(11) 0.15069(8) 0.0405(4) Uani 1 1 d . . .
H27A H 0.0160 0.7140 0.1184 0.061 Uiso 1 1 calc R . .
H27B H -0.0012 0.6764 0.1906 0.061 Uiso 1 1 calc R . .
H27C H 0.0195 0.6125 0.1313 0.061 Uiso 1 1 calc R . .
C28 C 0.13054(9) 0.60963(10) 0.22040(7) 0.0384(4) Uani 1 1 d . . .
H28A H 0.1228 0.5520 0.2021 0.058 Uiso 1 1 calc R . .
H28B H 0.1009 0.6168 0.2604 0.058 Uiso 1 1 calc R . .
H28C H 0.1820 0.6168 0.2317 0.058 Uiso 1 1 calc R . .
C29 C 0.15944(7) 0.59404(8) 0.07297(7) 0.0266(3) Uani 1 1 d . . .
H29 H 0.1158 0.5604 0.0872 0.032 Uiso 1 1 calc R . .
C30 C 0.15078(8) 0.60783(9) -0.00128(7) 0.0329(3) Uani 1 1 d . . .
H30A H 0.1058 0.6397 -0.0099 0.049 Uiso 1 1 calc R . .
H30B H 0.1487 0.5519 -0.0237 0.049 Uiso 1 1 calc R . .
H30C H 0.1923 0.6407 -0.0181 0.049 Uiso 1 1 calc R . .
C31 C 0.22504(8) 0.53709(9) 0.08847(8) 0.0340(3) Uani 1 1 d . . .
H31A H 0.2683 0.5605 0.0665 0.051 Uiso 1 1 calc R . .
H31B H 0.2159 0.4786 0.0723 0.051 Uiso 1 1 calc R . .
H31C H 0.2330 0.5356 0.1365 0.051 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'
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
C1 N1 C2 129.99(10) . . ?
N2 C1 N3 120.57(11) . . ?
N2 C1 N1 122.02(11) . . ?
N3 C1 N1 117.42(10) . . ?
C1 N2 C14 120.55(10) . . ?
C7 C2 C3 121.49(12) . . ?
C7 C2 N1 120.86(11) . . ?
C3 C2 N1 117.58(11) . . ?
C1 N3 C26 121.22(10) . . ?
C1 N3 C29 119.88(10) . . ?
C26 N3 C29 115.88(10) . . ?
C4 C3 C2 118.15(12) . . ?
C4 C3 C8 119.72(12) . . ?
C2 C3 C8 122.13(11) . . ?
C5 C4 C3 121.12(13) . . ?
C4 C5 C6 119.86(13) . . ?
C5 C6 C7 121.80(13) . . ?
C6 C7 C2 117.56(12) . . ?
C6 C7 C11 119.89(12) . . ?
C2 C7 C11 122.48(11) . . ?
C9 C8 C10 110.25(14) . . ?
C9 C8 C3 111.35(12) . . ?
C10 C8 C3 112.69(12) . . ?
C7 C11 C13 113.48(12) . . ?
C7 C11 C12 110.18(11) . . ?
C13 C11 C12 109.94(12) . . ?
C19 C14 N2 119.70(11) . . ?
C19 C14 C15 120.08(12) . . ?
N2 C14 C15 119.95(11) . . ?
C16 C15 C14 118.58(12) . . ?
C16 C15 C20 120.84(12) . . ?
C14 C15 C20 120.41(11) . . ?
C17 C16 C15 121.40(13) . . ?
C18 C17 C16 119.75(13) . . ?
C17 C18 C19 121.45(13) . . ?
C18 C19 C14 118.63(12) . . ?
C18 C19 C23 121.87(12) . . ?
C14 C19 C23 119.33(12) . . ?
C15 C20 C21 113.84(12) . . ?
C15 C20 C22 109.52(11) . . ?
C21 C20 C22 110.36(12) . . ?
C19 C23 C25 114.29(12) . . ?
C19 C23 C24 108.88(11) . . ?
C25 C23 C24 110.26(12) . . ?
N3 C26 C27 111.75(12) . . ?
N3 C26 C28 113.04(11) . . ?
C27 C26 C28 111.35(12) . . ?
N3 C29 C30 111.53(11) . . ?
N3 C29 C31 115.67(11) . . ?
C30 C29 C31 111.44(12) . . ?
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
N1 C1 1.3910(16) . ?
N1 C2 1.4379(16) . ?
C1 N2 1.2911(16) . ?
C1 N3 1.3807(16) . ?
N2 C14 1.4139(16) . ?
C2 C7 1.4069(18) . ?
C2 C3 1.4072(19) . ?
N3 C26 1.4746(16) . ?
N3 C29 1.4848(16) . ?
C3 C4 1.3946(19) . ?
C3 C8 1.5255(19) . ?
C4 C5 1.379(2) . ?
C5 C6 1.380(2) . ?
C6 C7 1.3930(19) . ?
C7 C11 1.5195(19) . ?
C8 C9 1.515(2) . ?
C8 C10 1.522(2) . ?
C11 C13 1.528(2) . ?
C11 C12 1.529(2) . ?
C14 C19 1.4134(18) . ?
C14 C15 1.4139(18) . ?
C15 C16 1.3950(18) . ?
C15 C20 1.5190(18) . ?
C16 C17 1.381(2) . ?
C17 C18 1.378(2) . ?
C18 C19 1.3946(19) . ?
C19 C23 1.515(2) . ?
C20 C21 1.522(2) . ?
C20 C22 1.532(2) . ?
C23 C25 1.5334(19) . ?
C23 C24 1.535(2) . ?
C26 C27 1.525(2) . ?
C26 C28 1.5269(19) . ?
C29 C30 1.521(2) . ?
C29 C31 1.5290(19) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 30652886
