#------------------------------------------------------------------------------
#$Date: 2025-08-21 14:03:24 +0200 (Thu 21 de Aug de 2025) $
#$Revision: 301848 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/61/7026178.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_7026178
loop_
_publ_author_name
'Brown, Christopher C.'
'Glotzbach, Christoph'
'Stephan, Douglas W.'
_publ_section_title
;
 Ag(I) and Au(I) complexes of sterically crowded cyclic phosphinimine
 ligands.
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9626
_journal_page_last               9632
_journal_paper_doi               10.1039/c0dt00261e
_journal_volume                  39
_journal_year                    2010
_chemical_formula_sum            'C25 H20 N P'
_chemical_formula_weight         365.39
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 90.314(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.9681(5)
_cell_length_b                   18.5680(6)
_cell_length_c                   6.9944(2)
_cell_measurement_temperature    150(2)
_cell_volume                     1943.91(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.951
_diffrn_measured_fraction_theta_max 0.951
_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  0.0357
_diffrn_reflns_av_sigmaI/netI    0.0417
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            19952
_diffrn_reflns_theta_full        29.88
_diffrn_reflns_theta_max         29.88
_diffrn_reflns_theta_min         1.36
_exptl_absorpt_coefficient_mu    0.150
_exptl_absorpt_correction_T_max  0.9563
_exptl_absorpt_correction_T_min  0.9355
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.249
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.316
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    fixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         5334
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0470
_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)+(0.0498P)²+0.8152P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1148
_refine_ls_wR_factor_ref         0.1231
_reflns_number_gt                4028
_reflns_number_total             5334
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0dt00261e.txt
_cod_data_source_block           Ph2CNPPh2
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7026178
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -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
P1 P 0.75719(3) 0.49857(2) 0.74539(6) 0.02320(11) Uani 1 1 d .
N1 N 0.78855(9) 0.44643(7) 0.55386(19) 0.0246(3) Uani 1 1 d .
C1 C 0.68078(11) 0.56397(8) 0.6344(2) 0.0233(3) Uani 1 1 d .
C2 C 0.61628(11) 0.54267(9) 0.5020(2) 0.0264(3) Uani 1 1 d .
H2A H 0.6096 0.4930 0.4722 0.032 Uiso 1 1 calc R
C3 C 0.56157(12) 0.59312(10) 0.4129(3) 0.0329(4) Uani 1 1 d .
H3A H 0.5181 0.5781 0.3218 0.040 Uiso 1 1 calc R
C4 C 0.57086(14) 0.66555(10) 0.4576(3) 0.0381(4) Uani 1 1 d .
H4A H 0.5333 0.7002 0.3977 0.046 Uiso 1 1 calc R
C5 C 0.63438(14) 0.68747(9) 0.5888(3) 0.0402(5) Uani 1 1 d .
H5A H 0.6405 0.7371 0.6190 0.048 Uiso 1 1 calc R
C6 C 0.68963(13) 0.63681(9) 0.6772(3) 0.0319(4) Uani 1 1 d .
H6A H 0.7335 0.6521 0.7671 0.038 Uiso 1 1 calc R
C7 C 0.67623(11) 0.43667(8) 0.8523(2) 0.0233(3) Uani 1 1 d .
C8 C 0.67080(12) 0.36371(9) 0.8070(2) 0.0293(4) Uani 1 1 d .
H8A H 0.7071 0.3446 0.7082 0.035 Uiso 1 1 calc R
C9 C 0.61281(13) 0.31858(9) 0.9051(3) 0.0347(4) Uani 1 1 d .
H9A H 0.6101 0.2688 0.8741 0.042 Uiso 1 1 calc R
C10 C 0.55899(13) 0.34609(10) 1.0479(3) 0.0345(4) Uani 1 1 d .
H10A H 0.5190 0.3153 1.1142 0.041 Uiso 1 1 calc R
C11 C 0.56342(13) 0.41852(10) 1.0942(2) 0.0330(4) Uani 1 1 d .
H11A H 0.5264 0.4375 1.1918 0.040 Uiso 1 1 calc R
C12 C 0.62203(12) 0.46332(9) 0.9978(2) 0.0285(4) Uani 1 1 d .
H12A H 0.6253 0.5128 1.0312 0.034 Uiso 1 1 calc R
C13 C 0.82879(10) 0.47130(8) 0.4066(2) 0.0217(3) Uani 1 1 d .
C14 C 0.85296(11) 0.42025(8) 0.2509(2) 0.0219(3) Uani 1 1 d .
C15 C 0.81487(12) 0.35155(9) 0.2444(2) 0.0270(3) Uani 1 1 d .
H15A H 0.7712 0.3383 0.3360 0.032 Uiso 1 1 calc R
C16 C 0.84023(13) 0.30281(9) 0.1060(3) 0.0319(4) Uani 1 1 d .
H16A H 0.8140 0.2562 0.1029 0.038 Uiso 1 1 calc R
C17 C 0.90375(12) 0.32138(9) -0.0286(3) 0.0313(4) Uani 1 1 d .
H17A H 0.9217 0.2875 -0.1225 0.038 Uiso 1 1 calc R
C18 C 0.94082(12) 0.38923(9) -0.0255(3) 0.0322(4) Uani 1 1 d .
H18A H 0.9841 0.4023 -0.1183 0.039 Uiso 1 1 calc R
C19 C 0.91523(12) 0.43867(9) 0.1125(2) 0.0278(4) Uani 1 1 d .
H19A H 0.9405 0.4856 0.1125 0.033 Uiso 1 1 calc R
C20 C 0.85492(11) 0.54909(8) 0.3854(2) 0.0227(3) Uani 1 1 d .
C21 C 0.81655(12) 0.59295(9) 0.2470(2) 0.0276(4) Uani 1 1 d .
H21A H 0.7753 0.5732 0.1574 0.033 Uiso 1 1 calc R
C22 C 0.83829(13) 0.66580(9) 0.2390(3) 0.0343(4) Uani 1 1 d .
H22A H 0.8107 0.6959 0.1462 0.041 Uiso 1 1 calc R
C23 C 0.90013(14) 0.69439(9) 0.3660(3) 0.0372(4) Uani 1 1 d .
H23A H 0.9150 0.7441 0.3602 0.045 Uiso 1 1 calc R
C24 C 0.94031(13) 0.65049(10) 0.5013(3) 0.0358(4) Uani 1 1 d .
H24A H 0.9837 0.6698 0.5866 0.043 Uiso 1 1 calc R
C25 C 0.91714(11) 0.57819(9) 0.5123(2) 0.0291(4) Uani 1 1 d .
H25A H 0.9439 0.5484 0.6071 0.035 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
N1 P1 C7 98.54(7)
N1 P1 C1 102.40(7)
C7 P1 C1 100.10(7)
C13 N1 P1 123.66(12)
C6 C1 C2 118.98(15)
C6 C1 P1 119.54(13)
C2 C1 P1 121.43(12)
C3 C2 C1 120.80(16)
C3 C2 H2A 119.6
C1 C2 H2A 119.6
C4 C3 C2 119.60(18)
C4 C3 H3A 120.2
C2 C3 H3A 120.2
C5 C4 C3 120.27(17)
C5 C4 H4A 119.9
C3 C4 H4A 119.9
C4 C5 C6 120.06(17)
C4 C5 H5A 120.0
C6 C5 H5A 120.0
C1 C6 C5 120.29(17)
C1 C6 H6A 119.9
C5 C6 H6A 119.9
C8 C7 C12 118.48(15)
C8 C7 P1 123.72(12)
C12 C7 P1 117.60(12)
C9 C8 C7 120.66(16)
C9 C8 H8A 119.7
C7 C8 H8A 119.7
C10 C9 C8 120.07(16)
C10 C9 H9A 120.0
C8 C9 H9A 120.0
C9 C10 C11 119.97(16)
C9 C10 H10A 120.0
C11 C10 H10A 120.0
C10 C11 C12 119.90(16)
C10 C11 H11A 120.0
C12 C11 H11A 120.0
C11 C12 C7 120.92(16)
C11 C12 H12A 119.5
C7 C12 H12A 119.5
N1 C13 C14 118.36(14)
N1 C13 C20 123.28(14)
C14 C13 C20 118.34(13)
C19 C14 C15 118.48(14)
C19 C14 C13 121.25(14)
C15 C14 C13 120.25(14)
C16 C15 C14 120.49(16)
C16 C15 H15A 119.8
C14 C15 H15A 119.8
C15 C16 C17 120.39(16)
C15 C16 H16A 119.8
C17 C16 H16A 119.8
C18 C17 C16 119.70(16)
C18 C17 H17A 120.2
C16 C17 H17A 120.2
C17 C18 C19 120.22(16)
C17 C18 H18A 119.9
C19 C18 H18A 119.9
C18 C19 C14 120.69(15)
C18 C19 H19A 119.7
C14 C19 H19A 119.7
C21 C20 C25 119.35(15)
C21 C20 C13 121.71(14)
C25 C20 C13 118.90(14)
C20 C21 C22 120.16(17)
C20 C21 H21A 119.9
C22 C21 H21A 119.9
C23 C22 C21 120.14(17)
C23 C22 H22A 119.9
C21 C22 H22A 119.9
C24 C23 C22 119.94(16)
C24 C23 H23A 120.0
C22 C23 H23A 120.0
C23 C24 C25 119.97(17)
C23 C24 H24A 120.0
C25 C24 H24A 120.0
C24 C25 C20 120.40(17)
C24 C25 H25A 119.8
C20 C25 H25A 119.8
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
P1 N1 1.7203(14)
P1 C7 1.8327(16)
P1 C1 1.8373(16)
N1 C13 1.282(2)
C1 C6 1.392(2)
C1 C2 1.392(2)
C2 C3 1.389(2)
C2 H2A 0.9500
C3 C4 1.388(3)
C3 H3A 0.9500
C4 C5 1.379(3)
C4 H4A 0.9500
C5 C6 1.395(3)
C5 H5A 0.9500
C6 H6A 0.9500
C7 C8 1.393(2)
C7 C12 1.396(2)
C8 C9 1.390(2)
C8 H8A 0.9500
C9 C10 1.384(3)
C9 H9A 0.9500
C10 C11 1.385(3)
C10 H10A 0.9500
C11 C12 1.387(2)
C11 H11A 0.9500
C12 H12A 0.9500
C13 C14 1.490(2)
C13 C20 1.504(2)
C14 C19 1.390(2)
C14 C15 1.398(2)
C15 C16 1.380(2)
C15 H15A 0.9500
C16 C17 1.385(3)
C16 H16A 0.9500
C17 C18 1.377(2)
C17 H17A 0.9500
C18 C19 1.388(2)
C18 H18A 0.9500
C19 H19A 0.9500
C20 C21 1.387(2)
C20 C25 1.392(2)
C21 C22 1.392(2)
C21 H21A 0.9500
C22 C23 1.385(3)
C22 H22A 0.9500
C23 C24 1.384(3)
C23 H23A 0.9500
C24 C25 1.389(2)
C24 H24A 0.9500
C25 H25A 0.9500
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 14270150
