#------------------------------------------------------------------------------
#$Date: 2016-03-26 14:21:19 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180258 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/44/7114422.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_7114422
loop_
_publ_author_name
'Coles, Martyn P.'
'Hitchcock, Peter B.'
_publ_section_title
;
 Variable coordination chemistry of the phospha(iii)guanidinate anion;
 application as a metal-functionalised phosphine ligandElectronic
 supplementary information (ESI) available: simulated and observed NMR
 spectra. See http://www.rsc.org/suppdata/cc/b2/b209026k/
;
_journal_issue                   23
_journal_name_full               'Chemical Communications'
_journal_page_first              2794
_journal_paper_doi               10.1039/b209026k
_journal_year                    2002
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C21 H30 Al1 N2 P1'
_chemical_formula_sum            'C21 H30 Al N2 P'
_chemical_formula_weight         368.42
_chemical_name_common            '[AlMe2{(NiPr)2CPPh2}]'
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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_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             2002-01-04T11:46:07-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 107.443(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.0218(9)
_cell_length_b                   8.3303(6)
_cell_length_c                   17.6419(9)
_cell_measurement_reflns_used    10071
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.986
_cell_measurement_theta_min      4.076
_cell_measurement_wavelength     0.71073
_cell_volume                     2246.3(2)
_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 0.987
_diffrn_measured_fraction_theta_max 0.987
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_av_unetI/netI     0.0438
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9341
_diffrn_reflns_theta_full        23.02
_diffrn_reflns_theta_max         23.02
_diffrn_reflns_theta_min         4.23
_exptl_absorpt_coefficient_mu    0.167
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.089
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.255
_refine_diff_density_min         -0.259
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3095
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0408
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0357P)²+1.4909P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0957
_refine_ls_wR_factor_ref         0.1009
_reflns_number_gt                2623
_reflns_number_total             3095
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b209026k.txt
_cod_data_source_block           jan202
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7114422
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
P P 0.98914(4) 0.15778(7) 0.32931(3) 0.02849(19) Uani 1 1 d .
Al Al 1.05867(5) 0.46187(9) 0.16642(4) 0.0357(2) Uani 1 1 d .
N1 N 1.02252(13) 0.2512(2) 0.18913(11) 0.0343(5) Uani 1 1 d .
N2 N 1.05219(12) 0.4498(2) 0.27359(11) 0.0325(5) Uani 1 1 d .
C1 C 1.02517(14) 0.2975(3) 0.26236(13) 0.0288(5) Uani 1 1 d .
C2 C 1.00808(15) 0.0882(3) 0.15664(13) 0.0346(6) Uani 1 1 d .
H2 H 0.9831 0.0209 0.1914 0.042 Uiso 1 1 calc R
C3 C 1.09435(18) 0.0165(4) 0.15517(18) 0.0588(8) Uani 1 1 d .
H3A H 1.1346 0.0129 0.2093 0.088 Uiso 1 1 calc R
H3B H 1.1197 0.0826 0.1217 0.088 Uiso 1 1 calc R
H3C H 1.0846 -0.0927 0.1335 0.088 Uiso 1 1 calc R
C4 C 0.94334(17) 0.0945(3) 0.07401(15) 0.0488(7) Uani 1 1 d .
H4A H 0.8879 0.1399 0.0769 0.073 Uiso 1 1 calc R
H4B H 0.9333 -0.0143 0.0520 0.073 Uiso 1 1 calc R
H4C H 0.9670 0.1619 0.0398 0.073 Uiso 1 1 calc R
C5 C 1.05883(17) 0.5499(3) 0.34315(14) 0.0381(6) Uani 1 1 d .
H5 H 1.0251 0.4989 0.3761 0.046 Uiso 1 1 calc R
C6 C 1.0197(2) 0.7134(3) 0.31490(17) 0.0581(8) Uani 1 1 d .
H6A H 0.9583 0.7006 0.2835 0.087 Uiso 1 1 calc R
H6B H 1.0522 0.7632 0.2820 0.087 Uiso 1 1 calc R
H6C H 1.0234 0.7819 0.3610 0.087 Uiso 1 1 calc R
C7 C 1.15440(19) 0.5664(4) 0.39273(16) 0.0569(8) Uani 1 1 d .
H7A H 1.1784 0.4600 0.4107 0.085 Uiso 1 1 calc R
H7B H 1.1584 0.6345 0.4389 0.085 Uiso 1 1 calc R
H7C H 1.1878 0.6151 0.3604 0.085 Uiso 1 1 calc R
C8 C 1.17570(18) 0.4768(4) 0.15516(18) 0.0655(9) Uani 1 1 d .
H8A H 1.1716 0.4825 0.0987 0.098 Uiso 1 1 calc R
H8B H 1.2097 0.3820 0.1789 0.098 Uiso 1 1 calc R
H8C H 1.2047 0.5736 0.1822 0.098 Uiso 1 1 calc R
C9 C 0.96150(17) 0.5857(3) 0.09533(15) 0.0467(7) Uani 1 1 d .
H9A H 0.9679 0.5882 0.0418 0.070 Uiso 1 1 calc R
H9B H 0.9626 0.6956 0.1154 0.070 Uiso 1 1 calc R
H9C H 0.9057 0.5349 0.0934 0.070 Uiso 1 1 calc R
C10 C 0.88971(14) 0.2571(3) 0.33491(12) 0.0279(5) Uani 1 1 d .
C11 C 0.84488(15) 0.3713(3) 0.28012(14) 0.0360(6) Uani 1 1 d .
H11 H 0.8708 0.4134 0.2424 0.043 Uiso 1 1 calc R
C12 C 0.76274(16) 0.4240(3) 0.28007(15) 0.0466(7) Uani 1 1 d .
H12 H 0.7324 0.5008 0.2419 0.056 Uiso 1 1 calc R
C13 C 0.72518(16) 0.3657(3) 0.33492(16) 0.0497(7) Uani 1 1 d .
H13 H 0.6691 0.4027 0.3348 0.060 Uiso 1 1 calc R
C14 C 0.76869(16) 0.2534(3) 0.39028(15) 0.0437(7) Uani 1 1 d .
H14 H 0.7428 0.2140 0.4285 0.052 Uiso 1 1 calc R
C15 C 0.84991(15) 0.1986(3) 0.38995(14) 0.0358(6) Uani 1 1 d .
H15 H 0.8792 0.1200 0.4276 0.043 Uiso 1 1 calc R
C16 C 1.07133(14) 0.1919(3) 0.42530(13) 0.0292(5) Uani 1 1 d .
C17 C 1.15290(15) 0.1230(3) 0.43378(14) 0.0379(6) Uani 1 1 d .
H17 H 1.1621 0.0625 0.3913 0.045 Uiso 1 1 calc R
C18 C 1.22051(16) 0.1418(3) 0.50347(16) 0.0478(7) Uani 1 1 d .
H18 H 1.2761 0.0958 0.5083 0.057 Uiso 1 1 calc R
C19 C 1.20768(17) 0.2269(3) 0.56603(15) 0.0478(7) Uani 1 1 d .
H19 H 1.2545 0.2407 0.6136 0.057 Uiso 1 1 calc R
C20 C 1.12664(16) 0.2918(3) 0.55929(14) 0.0448(7) Uani 1 1 d .
H20 H 1.1173 0.3484 0.6028 0.054 Uiso 1 1 calc R
C21 C 1.05866(15) 0.2752(3) 0.48943(13) 0.0352(6) Uani 1 1 d .
H21 H 1.0031 0.3208 0.4852 0.042 Uiso 1 1 calc R
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
C10 P C16 106.12(10)
C10 P C1 101.07(10)
C16 P C1 102.44(10)
N2 Al N1 68.95(8)
N2 Al C8 116.11(11)
N1 Al C8 115.96(13)
N2 Al C9 112.75(10)
N1 Al C9 112.30(10)
C8 Al C9 120.14(13)
C1 N1 C2 126.97(19)
C1 N1 Al 90.76(14)
C2 N1 Al 141.69(15)
C1 N2 C5 127.26(19)
C1 N2 Al 90.82(13)
C5 N2 Al 141.50(15)
N2 C1 N1 109.43(19)
N2 C1 P 130.21(16)
N1 C1 P 120.30(17)
N1 C2 C3 109.6(2)
N1 C2 C4 109.1(2)
C3 C2 C4 111.2(2)
N2 C5 C6 108.5(2)
N2 C5 C7 109.9(2)
C6 C5 C7 110.6(2)
C11 C10 C15 118.2(2)
C11 C10 P 123.33(17)
C15 C10 P 117.83(17)
C12 C11 C10 120.6(2)
C13 C12 C11 120.3(2)
C12 C13 C14 120.2(2)
C13 C14 C15 119.9(2)
C14 C15 C10 120.9(2)
C21 C16 C17 118.6(2)
C21 C16 P 126.13(17)
C17 C16 P 115.28(17)
C18 C17 C16 120.5(2)
C19 C18 C17 120.4(2)
C20 C19 C18 119.7(2)
C19 C20 C21 120.4(2)
C20 C21 C16 120.4(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
P C10 1.824(2)
P C16 1.829(2)
P C1 1.869(2)
Al N2 1.9270(19)
Al N1 1.928(2)
Al C8 1.948(3)
Al C9 1.972(3)
N1 C1 1.337(3)
N1 C2 1.465(3)
N2 C1 1.336(3)
N2 C5 1.461(3)
C2 C3 1.513(3)
C2 C4 1.516(3)
C5 C6 1.520(3)
C5 C7 1.525(4)
C10 C11 1.392(3)
C10 C15 1.399(3)
C11 C12 1.387(3)
C12 C13 1.373(4)
C13 C14 1.380(4)
C14 C15 1.381(3)
C16 C21 1.393(3)
C16 C17 1.394(3)
C17 C18 1.383(3)
C18 C19 1.378(4)
C19 C20 1.378(4)
C20 C21 1.386(3)
