#------------------------------------------------------------------------------
#$Date: 2017-10-14 22:27:35 +0300 (Sat, 14 Oct 2017) $
#$Revision: 202017 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/41/7014164.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_7014164
loop_
_publ_author_name
'Mokuolu, Q. Folashade'
'Duckmanton, Paul A.'
'Hitchcock, Peter B.'
'Wilson, Claire'
'Blake, Alexander J.'
'Shukla, Lena'
'Love, Jason B.'
_publ_section_title
;
 Early-late, mixed-metal compounds supported by amidophosphine ligands.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1960
_journal_page_last               1970
_journal_paper_doi               10.1039/b402409e
_journal_year                    2004
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C27 H34 N O P'
_chemical_formula_structural     'C27 H34 N O P'
_chemical_formula_sum            'C27 H34 N O P'
_chemical_formula_weight         419.52
_chemical_name_common            (Ph2P(O)C6H4NHCH(tBu)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/cifdics/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1
_audit_creation_date             2001-01-25T09:55:46-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                114.750(3)
_cell_angle_beta                 102.930(4)
_cell_angle_gamma                92.017(4)
_cell_formula_units_Z            2
_cell_length_a                   8.5913(5)
_cell_length_b                   11.8796(8)
_cell_length_c                   13.3003(9)
_cell_measurement_reflns_used    4587
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.534
_cell_measurement_theta_min      3.705
_cell_measurement_wavelength     0.71073
_cell_volume                     1188.69(14)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_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 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device       KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_av_unetI/netI     0.057
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7517
_diffrn_reflns_theta_full        23.56
_diffrn_reflns_theta_max         23.56
_diffrn_reflns_theta_min         3.71
_exptl_absorpt_coefficient_mu    0.134
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.172
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             452
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.214
_refine_diff_density_min         -0.35
_refine_diff_density_rms         0.04
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         3507
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0597
_refine_ls_R_factor_gt           0.0437
_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)+(0.0313P)²+0.6081P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0957
_refine_ls_wR_factor_ref         0.1037
_reflns_number_gt                2826
_reflns_number_total             3507
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b402409e.txt
_cod_data_source_block           jan601
_cod_original_cell_volume        1188.69(13)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7014164
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
_atom_site_disorder_assembly
_atom_site_disorder_group
P P 0.24616(6) 0.73369(5) 0.03392(5) 0.02140(17) Uani 1 1 d . . .
O O 0.18095(16) 0.68137(13) 0.10297(12) 0.0240(3) Uani 1 1 d . . .
N N -0.1833(2) 0.39053(17) -0.29884(16) 0.0337(5) Uani 1 1 d . . .
H1 H -0.189(3) 0.364(2) -0.247(2) 0.039(7) Uiso 1 1 d . . .
C1 C 0.1412(2) 0.65461(18) -0.11648(17) 0.0217(5) Uani 1 1 d . . .
C2 C 0.0227(2) 0.55374(19) -0.15215(18) 0.0229(5) Uani 1 1 d . . .
H2 H 0.0018 0.5272 -0.0977 0.028 Uiso 1 1 calc R . .
C3 C -0.0674(3) 0.48966(19) -0.26802(18) 0.0268(5) Uani 1 1 d . . .
C4 C -0.0333(3) 0.5338(2) -0.3447(2) 0.0350(6) Uani 1 1 d . . .
H4 H -0.0936 0.4946 -0.4229 0.042 Uiso 1 1 calc R . .
C5 C 0.0869(3) 0.6335(2) -0.3080(2) 0.0351(6) Uani 1 1 d . . .
H5 H 0.1087 0.6605 -0.362 0.042 Uiso 1 1 calc R . .
C6 C 0.1760(3) 0.6949(2) -0.19509(19) 0.0289(5) Uani 1 1 d . . .
H6 H 0.2589 0.7628 -0.1713 0.035 Uiso 1 1 calc R . .
C7 C 0.2294(2) 0.89831(19) 0.08036(18) 0.0237(5) Uani 1 1 d . . .
C8 C 0.1142(3) 0.9459(2) 0.1394(2) 0.0347(6) Uani 1 1 d . . .
H8 H 0.0496 0.8928 0.1561 0.042 Uiso 1 1 calc R . .
C9 C 0.0932(3) 1.0699(2) 0.1738(2) 0.0444(7) Uani 1 1 d . . .
H9 H 0.0139 1.1016 0.2139 0.053 Uiso 1 1 calc R . .
C10 C 0.1859(3) 1.1483(2) 0.1506(2) 0.0402(6) Uani 1 1 d . . .
H10 H 0.1706 1.2336 0.1748 0.048 Uiso 1 1 calc R . .
C11 C 0.3006(3) 1.1030(2) 0.0925(2) 0.0432(7) Uani 1 1 d . . .
H11 H 0.3654 1.1567 0.0766 0.052 Uiso 1 1 calc R . .
C12 C 0.3211(3) 0.9780(2) 0.0572(2) 0.0373(6) Uani 1 1 d . . .
H12 H 0.3998 0.9466 0.0164 0.045 Uiso 1 1 calc R . .
C13 C 0.4569(2) 0.72182(19) 0.04195(18) 0.0228(5) Uani 1 1 d . . .
C14 C 0.5054(3) 0.6209(2) -0.0396(2) 0.0296(5) Uani 1 1 d . . .
H14 H 0.4275 0.5623 -0.1062 0.036 Uiso 1 1 calc R . .
C15 C 0.6665(3) 0.6055(2) -0.0242(2) 0.0334(6) Uani 1 1 d . . .
H15 H 0.6987 0.5363 -0.0802 0.04 Uiso 1 1 calc R . .
C16 C 0.7802(3) 0.6897(2) 0.0714(2) 0.0353(6) Uani 1 1 d . . .
H16 H 0.8906 0.6785 0.0817 0.042 Uiso 1 1 calc R . .
C17 C 0.7338(3) 0.7911(2) 0.1530(2) 0.0374(6) Uani 1 1 d . . .
H17 H 0.8124 0.8496 0.2192 0.045 Uiso 1 1 calc R . .
C18 C 0.5729(3) 0.8071(2) 0.13795(19) 0.0321(6) Uani 1 1 d . . .
H18 H 0.5415 0.877 0.1938 0.039 Uiso 1 1 calc R . .
C19 C -0.2854(3) 0.3127(2) -0.4144(2) 0.0398(6) Uani 1 1 d . . .
H19 H -0.2594 0.3531 -0.4624 0.048 Uiso 1 1 calc R . .
C20 C -0.2269(4) 0.1814(2) -0.4627(2) 0.0496(7) Uani 1 1 d . . .
C21 C -0.2577(5) 0.1030(3) -0.4011(3) 0.0802(12) Uani 1 1 d . . .
H21C H -0.3743 0.0814 -0.4154 0.12 Uiso 1 1 calc R . .
H21B H -0.2094 0.1512 -0.3185 0.12 Uiso 1 1 calc R . .
H21A H -0.2093 0.0261 -0.4299 0.12 Uiso 1 1 calc R . .
C22 C -0.3027(4) 0.1042(3) -0.5921(3) 0.0770(11) Uani 1 1 d . . .
H22C H -0.2526 0.0281 -0.6202 0.116 Uiso 1 1 calc R . .
H22B H -0.2851 0.1541 -0.6325 0.116 Uiso 1 1 calc R . .
H22A H -0.4189 0.0812 -0.606 0.116 Uiso 1 1 calc R . .
C23 C -0.0447(4) 0.2038(3) -0.4485(3) 0.0672(9) Uani 1 1 d . . .
H23C H -0.0046 0.123 -0.4778 0.101 Uiso 1 1 calc R . .
H23B H 0.0107 0.2528 -0.3671 0.101 Uiso 1 1 calc R . .
H23A H -0.0237 0.2497 -0.4916 0.101 Uiso 1 1 calc R . .
C24 C -0.4663(3) 0.3284(2) -0.4142(2) 0.0473(7) Uani 1 1 d . . .
C25 C -0.5816(4) 0.2649(3) -0.5356(3) 0.0742(10) Uani 1 1 d . . .
H25C H -0.5856 0.1738 -0.566 0.111 Uiso 1 1 calc R . .
H25B H -0.5427 0.2938 -0.5859 0.111 Uiso 1 1 calc R . .
H25A H -0.69 0.2866 -0.5323 0.111 Uiso 1 1 calc R . .
C26 C -0.5291(3) 0.2831(3) -0.3367(3) 0.0642(9) Uani 1 1 d . . .
H26C H -0.4608 0.3276 -0.258 0.096 Uiso 1 1 calc R . .
H26B H -0.5263 0.1929 -0.3642 0.096 Uiso 1 1 calc R . .
H26A H -0.6403 0.2997 -0.3384 0.096 Uiso 1 1 calc R . .
C27 C -0.4745(4) 0.4697(3) -0.3677(3) 0.0573(8) Uani 1 1 d . . .
H27C H -0.5864 0.4841 -0.3689 0.086 Uiso 1 1 calc R . .
H27B H -0.4359 0.5022 -0.4158 0.086 Uiso 1 1 calc R . .
H27A H -0.4065 0.513 -0.2887 0.086 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'
O O 0.0106 0.006 '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
O P C13 113.39(9) . . ?
O P C1 112.04(9) . . ?
C13 P C1 106.10(9) . . ?
O P C7 112.10(9) . . ?
C13 P C7 105.90(10) . . ?
C1 P C7 106.81(9) . . ?
C3 N C19 126.2(2) . . ?
C2 C1 C6 120.6(2) . . ?
C2 C1 P 118.15(15) . . ?
C6 C1 P 121.22(16) . . ?
C1 C2 C3 121.2(2) . . ?
N C3 C4 123.9(2) . . ?
N C3 C2 118.91(19) . . ?
C4 C3 C2 117.2(2) . . ?
C5 C4 C3 120.9(2) . . ?
C6 C5 C4 121.8(2) . . ?
C5 C6 C1 118.3(2) . . ?
C12 C7 C8 118.4(2) . . ?
C12 C7 P 123.63(16) . . ?
C8 C7 P 117.91(17) . . ?
C9 C8 C7 120.2(2) . . ?
C10 C9 C8 120.7(2) . . ?
C11 C10 C9 119.8(2) . . ?
C10 C11 C12 119.5(2) . . ?
C7 C12 C11 121.3(2) . . ?
C18 C13 C14 118.89(19) . . ?
C18 C13 P 119.36(15) . . ?
C14 C13 P 121.34(17) . . ?
C15 C14 C13 120.3(2) . . ?
C16 C15 C14 120.4(2) . . ?
C15 C16 C17 119.9(2) . . ?
C18 C17 C16 119.9(2) . . ?
C17 C18 C13 120.5(2) . . ?
N C19 C20 109.1(2) . . ?
N C19 C24 108.51(19) . . ?
C20 C19 C24 122.7(2) . . ?
C21 C20 C23 108.6(3) . . ?
C21 C20 C22 108.7(2) . . ?
C23 C20 C22 105.7(2) . . ?
C21 C20 C19 113.4(2) . . ?
C23 C20 C19 107.7(2) . . ?
C22 C20 C19 112.4(2) . . ?
C26 C24 C27 107.1(2) . . ?
C26 C24 C25 108.9(2) . . ?
C27 C24 C25 107.1(2) . . ?
C26 C24 C19 114.4(2) . . ?
C27 C24 C19 106.4(2) . . ?
C25 C24 C19 112.5(2) . . ?
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
P O 1.4924(15) . ?
P C13 1.803(2) . ?
P C1 1.805(2) . ?
P C7 1.810(2) . ?
N C3 1.370(3) . ?
N C19 1.462(3) . ?
C1 C2 1.385(3) . ?
C1 C6 1.400(3) . ?
C2 C3 1.413(3) . ?
C3 C4 1.404(3) . ?
C4 C5 1.382(3) . ?
C5 C6 1.379(3) . ?
C7 C12 1.383(3) . ?
C7 C8 1.390(3) . ?
C8 C9 1.380(3) . ?
C9 C10 1.376(3) . ?
C10 C11 1.374(3) . ?
C11 C12 1.388(3) . ?
C13 C18 1.388(3) . ?
C13 C14 1.392(3) . ?
C14 C15 1.384(3) . ?
C15 C16 1.372(3) . ?
C16 C17 1.386(3) . ?
C17 C18 1.383(3) . ?
C19 C20 1.568(4) . ?
C19 C24 1.572(4) . ?
C20 C21 1.526(4) . ?
C20 C23 1.535(4) . ?
C20 C22 1.536(4) . ?
C24 C26 1.529(4) . ?
C24 C27 1.537(4) . ?
C24 C25 1.539(4) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 21145471
