#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:11:33 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178639 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/50/4075056.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_4075056
loop_
_publ_author_name
'Mansfield, Natalie E.'
'Coles, Martyn P.'
'Avent, Anthony G.'
'Hitchcock, Peter B.'
_publ_section_title
;
 Coordination Chemistry of Isomeric Mixtures of Linked
 Di(phosphaguanidine) Compounds:  A Spectroscopic and
 Crystallographic Study
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              2470
_journal_paper_doi               10.1021/om060014z
_journal_volume                  25
_journal_year                    2006
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C40 H60 N4 P2'
_chemical_formula_sum            'C40 H60 N4 P2'
_chemical_formula_weight         658.86
_chemical_name_common            '[{-CH2P(Ph)C(NHcy)(Ncy)}2]'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2002-09-27T14:37:43-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                110.804(5)
_cell_angle_beta                 97.381(5)
_cell_angle_gamma                94.342(4)
_cell_formula_units_Z            1
_cell_length_a                   9.2204(7)
_cell_length_b                   10.0638(8)
_cell_length_c                   11.1221(9)
_cell_measurement_reflns_used    7908
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.722
_cell_measurement_theta_min      3.705
_cell_measurement_wavelength     0.71073
_cell_volume                     948.53(13)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0715
_diffrn_reflns_av_unetI/netI     0.0825
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5230
_diffrn_reflns_theta_full        22.89
_diffrn_reflns_theta_max         22.89
_diffrn_reflns_theta_min         3.98
_exptl_absorpt_coefficient_mu    0.147
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.153
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             358
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.258
_refine_diff_density_min         -0.217
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         2502
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0861
_refine_ls_R_factor_gt           0.0584
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0421P)²+0.6512P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1227
_refine_ls_wR_factor_ref         0.1353
_reflns_number_gt                1910
_reflns_number_total             2502
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060014zsi20060105_063055.cif
_cod_data_source_block           (1b)-sep2202
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4075056
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
P P 0.50648(10) 0.56670(9) 0.32723(9) 0.0310(3) Uani 1 1 d .
N1 N 0.7764(3) 0.7264(3) 0.3447(3) 0.0317(7) Uani 1 1 d .
N2 N 0.7483(3) 0.4911(3) 0.2061(3) 0.0342(7) Uani 1 1 d .
H2X H 0.691(5) 0.408(5) 0.176(4) 0.064(14) Uiso 1 1 d .
C1 C 0.6964(4) 0.6051(4) 0.2931(3) 0.0291(8) Uani 1 1 d .
C2 C 0.7208(4) 0.8516(3) 0.4315(3) 0.0319(8) Uani 1 1 d .
H2 H 0.6127 0.8279 0.4285 0.038 Uiso 1 1 calc R
C3 C 0.7453(4) 0.9743(4) 0.3832(3) 0.0370(9) Uani 1 1 d .
H3B H 0.6814 0.9499 0.2977 0.044 Uiso 1 1 calc R
H3A H 0.8491 0.9851 0.3701 0.044 Uiso 1 1 calc R
C4 C 0.7121(4) 1.1169(4) 0.4774(3) 0.0409(9) Uani 1 1 d .
H4B H 0.7397 1.1939 0.4454 0.049 Uiso 1 1 calc R
H4A H 0.6048 1.1115 0.4792 0.049 Uiso 1 1 calc R
C5 C 0.7944(4) 1.1548(4) 0.6143(4) 0.0454(10) Uani 1 1 d .
H5B H 0.7637 1.2436 0.6734 0.054 Uiso 1 1 calc R
H5A H 0.9017 1.1727 0.6151 0.054 Uiso 1 1 calc R
C6 C 0.7629(4) 1.0338(4) 0.6622(4) 0.0459(10) Uani 1 1 d .
H6B H 0.8213 1.0582 0.7501 0.055 Uiso 1 1 calc R
H6A H 0.6572 1.0227 0.6695 0.055 Uiso 1 1 calc R
C7 C 0.8006(4) 0.8938(4) 0.5712(3) 0.0399(9) Uani 1 1 d .
H7B H 0.7742 0.8171 0.6038 0.048 Uiso 1 1 calc R
H7A H 0.9083 0.9021 0.5717 0.048 Uiso 1 1 calc R
C8 C 0.9020(4) 0.4932(4) 0.1841(3) 0.0346(9) Uani 1 1 d .
H8 H 0.9324 0.5845 0.1719 0.042 Uiso 1 1 calc R
C9 C 1.0053(4) 0.4870(4) 0.2997(3) 0.0410(9) Uani 1 1 d .
H9B H 1.1087 0.5017 0.2868 0.049 Uiso 1 1 calc R
H9A H 0.992 0.5654 0.3802 0.049 Uiso 1 1 calc R
C10 C 0.9766(4) 0.3452(4) 0.3161(3) 0.0456(10) Uani 1 1 d .
H10B H 0.8764 0.3344 0.3372 0.055 Uiso 1 1 calc R
H10A H 1.0484 0.3437 0.3897 0.055 Uiso 1 1 calc R
C11 C 0.9898(4) 0.2204(4) 0.1925(3) 0.0450(10) Uani 1 1 d .
H11B H 0.9647 0.1289 0.2042 0.054 Uiso 1 1 calc R
H11A H 1.093 0.2253 0.1768 0.054 Uiso 1 1 calc R
C12 C 0.8876(4) 0.2237(4) 0.0748(3) 0.0439(10) Uani 1 1 d .
H12B H 0.9054 0.1471 -0.0051 0.053 Uiso 1 1 calc R
H12A H 0.7838 0.2046 0.0848 0.053 Uiso 1 1 calc R
C13 C 0.9125(4) 0.3682(4) 0.0603(3) 0.0399(9) Uani 1 1 d .
H13B H 1.0112 0.3801 0.0366 0.048 Uiso 1 1 calc R
H13A H 0.8382 0.3697 -0.0117 0.048 Uiso 1 1 calc R
C14 C 0.4417(3) 0.3908(3) 0.1998(3) 0.0270(8) Uani 1 1 d .
C15 C 0.3689(4) 0.3902(4) 0.0815(3) 0.0361(9) Uani 1 1 d .
H15 H 0.357 0.4788 0.0714 0.043 Uiso 1 1 calc R
C16 C 0.3141(4) 0.2642(4) -0.0206(3) 0.0420(10) Uani 1 1 d .
H16 H 0.2663 0.2663 -0.1007 0.05 Uiso 1 1 calc R
C17 C 0.3283(4) 0.1348(4) -0.0070(3) 0.0448(10) Uani 1 1 d .
H17 H 0.2894 0.0476 -0.0772 0.054 Uiso 1 1 calc R
C18 C 0.3992(4) 0.1325(4) 0.1085(3) 0.0403(9) Uani 1 1 d .
H18 H 0.4093 0.0434 0.118 0.048 Uiso 1 1 calc R
C19 C 0.4557(4) 0.2588(4) 0.2107(3) 0.0340(8) Uani 1 1 d .
H19 H 0.5049 0.2556 0.2899 0.041 Uiso 1 1 calc R
C20 C 0.5661(4) 0.5213(4) 0.4715(3) 0.0356(9) Uani 1 1 d .
H20A H 0.6255 0.4408 0.4466 0.043 Uiso 1 1 calc R
H20B H 0.6295 0.6048 0.5394 0.043 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 0 '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
C14 P C20 102.64(15) .
C14 P C1 101.67(15) .
C20 P C1 96.55(14) .
C1 N1 C2 121.1(3) .
C1 N2 C8 123.3(3) .
N1 C1 N2 120.0(3) .
N1 C1 P 124.5(2) .
N2 C1 P 115.6(2) .
N1 C2 C3 108.3(3) .
N1 C2 C7 110.3(3) .
C3 C2 C7 110.5(3) .
C2 C3 C4 112.9(3) .
C5 C4 C3 112.3(3) .
C4 C5 C6 110.3(3) .
C7 C6 C5 111.6(3) .
C6 C7 C2 112.8(3) .
N2 C8 C13 109.3(3) .
N2 C8 C9 111.5(3) .
C13 C8 C9 110.5(3) .
C10 C9 C8 111.7(3) .
C9 C10 C11 111.2(3) .
C10 C11 C12 111.2(3) .
C13 C12 C11 111.3(3) .
C8 C13 C12 112.7(3) .
C19 C14 C15 117.4(3) .
C19 C14 P 126.2(2) .
C15 C14 P 116.4(2) .
C16 C15 C14 121.4(3) .
C15 C16 C17 120.1(3) .
C18 C17 C16 119.7(3) .
C17 C18 C19 120.4(3) .
C18 C19 C14 121.1(3) .
C20 C20 P 112.1(3) 2_666
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
P C14 1.828(3) .
P C20 1.849(3) .
P C1 1.880(3) .
N1 C1 1.273(4) .
N1 C2 1.464(4) .
N2 C1 1.376(4) .
N2 C8 1.469(4) .
C2 C3 1.525(4) .
C2 C7 1.525(5) .
C3 C4 1.527(5) .
C4 C5 1.513(5) .
C5 C6 1.516(5) .
C6 C7 1.510(5) .
C8 C13 1.519(5) .
C8 C9 1.522(5) .
C9 C10 1.510(5) .
C10 C11 1.524(5) .
C11 C12 1.524(5) .
C12 C13 1.523(5) .
C14 C19 1.390(4) .
C14 C15 1.395(5) .
C15 C16 1.373(5) .
C16 C17 1.377(5) .
C17 C18 1.373(5) .
C18 C19 1.379(5) .
C20 C20 1.543(6) 2_666
