#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/08/7010899.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_7010899
loop_
_publ_author_name
'Said, Musa'
'Thornton-Pett, Mark'
'Bochmann, Manfred'
_publ_section_title
;
 Titanium and zirconium complexes with sterically hindered
 aryl-substituted iminophosphoranato ligands
;
_journal_issue                   19
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2844
_journal_paper_doi               10.1039/b105038a
_journal_year                    2001
_chemical_formula_sum            'C38 H52 N4 P Zr'
_chemical_formula_weight         687.03
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                92.661(3)
_cell_angle_beta                 111.753(3)
_cell_angle_gamma                104.507(3)
_cell_formula_units_Z            2
_cell_length_a                   10.6664(6)
_cell_length_b                   13.6098(5)
_cell_length_c                   14.1992(8)
_cell_measurement_temperature    150(2)
_cell_volume                     1831.08(17)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1996)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1996)'
_computing_molecular_graphics    'ORTEX (McArdle, 1995)'
_computing_publication_material  'WC (Thornton-Pett, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type
'Nonius KappaCCD area detector diffractometer'
_diffrn_measurement_method
;
Detector set at 30mm from sample with different 2theta offsets 
1 degree phi exposures for chi=0 degree settings
1 degree omega exposures for chi=90 degree settings
;
_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  0.0658
_diffrn_reflns_av_sigmaI/netI    0.0697
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17202
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.44
_exptl_absorpt_coefficient_mu    0.374
_exptl_absorpt_correction_T_max  0.9707
_exptl_absorpt_correction_T_min  0.8928
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Using multiple and symmetry-related data measurements via the program SORTAV
See R.H. Blessing, Acta Cryst (1995), A51, 33-38 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             726
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.121
_refine_diff_density_min         -1.086
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         7079
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0632
_refine_ls_R_factor_gt           0.0528
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0835P)²+1.1427P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1392
_refine_ls_wR_factor_ref         0.1502
_reflns_number_gt                6024
_reflns_number_total             7079
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b105038a.txt
_cod_data_source_block           msp125a
_cod_original_cell_volume        1831.08(16)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7010899
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
Zr1 Zr 0.74174(3) 0.81720(2) 0.70715(2) 0.03421(13) Uani 1 1 d . . .
N1 N 0.8964(3) 0.72309(19) 0.7437(2) 0.0339(5) Uani 1 1 d . . .
C11 C 0.8753(3) 0.6170(2) 0.7569(2) 0.0345(6) Uani 1 1 d . . .
C12 C 0.8661(3) 0.5882(2) 0.8487(2) 0.0382(7) Uani 1 1 d . . .
C13 C 0.8338(4) 0.4849(3) 0.8585(3) 0.0437(8) Uani 1 1 d . . .
H13 H 0.8297 0.4661 0.9211 0.052 Uiso 1 1 calc R . .
C14 C 0.8074(4) 0.4080(2) 0.7800(3) 0.0430(8) Uani 1 1 d . . .
C15 C 0.8195(4) 0.4381(2) 0.6908(3) 0.0407(7) Uani 1 1 d . . .
H15 H 0.8039 0.3867 0.6368 0.049 Uiso 1 1 calc R . .
C16 C 0.8538(3) 0.5408(2) 0.6776(3) 0.0370(7) Uani 1 1 d . . .
C17 C 0.8900(5) 0.6682(3) 0.9354(3) 0.0496(9) Uani 1 1 d . . .
H17A H 0.8071 0.6934 0.9187 0.074 Uiso 1 1 calc R . .
H17B H 0.9729 0.7256 0.9456 0.074 Uiso 1 1 calc R . .
H17C H 0.9057 0.6377 0.9985 0.074 Uiso 1 1 calc R . .
C18 C 0.7658(4) 0.2957(3) 0.7914(3) 0.0505(9) Uani 1 1 d . . .
H18A H 0.8146 0.2876 0.8628 0.076 Uiso 1 1 calc R . .
H18B H 0.7921 0.2554 0.7466 0.076 Uiso 1 1 calc R . .
H18C H 0.6636 0.2713 0.7719 0.076 Uiso 1 1 calc R . .
C19 C 0.8654(4) 0.5673(3) 0.5783(3) 0.0448(8) Uani 1 1 d . . .
H19A H 0.9650 0.5936 0.5897 0.067 Uiso 1 1 calc R . .
H19B H 0.8178 0.6200 0.5548 0.067 Uiso 1 1 calc R . .
H19C H 0.8208 0.5057 0.5261 0.067 Uiso 1 1 calc R . .
P1 P 1.04643(8) 0.80735(6) 0.76482(6) 0.03201(19) Uani 1 1 d . . .
C111 C 1.1943(3) 0.7872(2) 0.8700(2) 0.0347(6) Uani 1 1 d . . .
C112 C 1.2158(4) 0.6908(2) 0.8837(3) 0.0417(7) Uani 1 1 d . . .
H112 H 1.1488 0.6308 0.8391 0.050 Uiso 1 1 calc R . .
C113 C 1.3363(4) 0.6835(3) 0.9633(3) 0.0486(8) Uani 1 1 d . . .
H113 H 1.3506 0.6181 0.9741 0.058 Uiso 1 1 calc R . .
C114 C 1.4358(4) 0.7714(3) 1.0271(3) 0.0505(9) Uani 1 1 d . . .
H114 H 1.5195 0.7662 1.0797 0.061 Uiso 1 1 calc R . .
C115 C 1.4134(4) 0.8662(3) 1.0143(3) 0.0453(8) Uani 1 1 d . . .
H115 H 1.4807 0.9260 1.0590 0.054 Uiso 1 1 calc R . .
C116 C 1.2933(3) 0.8742(2) 0.9366(3) 0.0383(7) Uani 1 1 d . . .
H116 H 1.2780 0.9397 0.9284 0.046 Uiso 1 1 calc R . .
C121 C 1.1013(3) 0.8072(2) 0.6584(2) 0.0355(6) Uani 1 1 d . . .
C122 C 1.2238(4) 0.7837(3) 0.6655(3) 0.0418(7) Uani 1 1 d . . .
H122 H 1.2829 0.7689 0.7286 0.050 Uiso 1 1 calc R . .
C123 C 1.2610(4) 0.7815(3) 0.5819(3) 0.0465(8) Uani 1 1 d . . .
H123 H 1.3439 0.7640 0.5873 0.056 Uiso 1 1 calc R . .
C124 C 1.1769(4) 0.8050(3) 0.4907(3) 0.0467(8) Uani 1 1 d . . .
H124 H 1.2018 0.8035 0.4331 0.056 Uiso 1 1 calc R . .
C125 C 1.0554(4) 0.8308(3) 0.4831(3) 0.0446(8) Uani 1 1 d . . .
H125 H 0.9988 0.8484 0.4206 0.054 Uiso 1 1 calc R . .
C126 C 1.0169(4) 0.8311(2) 0.5656(3) 0.0411(7) Uani 1 1 d . . .
H126 H 0.9330 0.8475 0.5595 0.049 Uiso 1 1 calc R . .
C1 C 1.0032(3) 0.9189(2) 0.7854(2) 0.0345(6) Uani 1 1 d . . .
C131 C 1.0749(3) 1.0255(2) 0.7786(2) 0.0335(6) Uani 1 1 d . . .
C132 C 1.0317(4) 1.1060(2) 0.8099(3) 0.0391(7) Uani 1 1 d . . .
H132 H 0.9574 1.0900 0.8334 0.047 Uiso 1 1 calc R . .
C133 C 1.0932(4) 1.2075(2) 0.8078(3) 0.0391(7) Uani 1 1 d . . .
H133 H 1.0609 1.2591 0.8308 0.047 Uiso 1 1 calc R . .
C134 C 1.2019(3) 1.2368(2) 0.7729(2) 0.0361(7) Uani 1 1 d . . .
C135 C 1.2442(3) 1.1570(2) 0.7411(2) 0.0368(7) Uani 1 1 d . . .
H135 H 1.3170 1.1730 0.7162 0.044 Uiso 1 1 calc R . .
C136 C 1.1841(3) 1.0549(2) 0.7445(2) 0.0361(6) Uani 1 1 d . . .
H136 H 1.2180 1.0035 0.7230 0.043 Uiso 1 1 calc R . .
C137 C 1.2667(4) 1.3503(2) 0.7710(3) 0.0424(7) Uani 1 1 d . . .
C138 C 1.3378(5) 1.4096(3) 0.8801(3) 0.0588(10) Uani 1 1 d . . .
H13A H 1.2665 1.4083 0.9084 0.088 Uiso 1 1 calc R . .
H13B H 1.3852 1.4810 0.8789 0.088 Uiso 1 1 calc R . .
H13C H 1.4072 1.3777 0.9230 0.088 Uiso 1 1 calc R . .
C139 C 1.3753(6) 1.3637(3) 0.7234(5) 0.0781(16) Uani 1 1 d . . .
H13D H 1.4103 1.4365 0.7193 0.117 Uiso 1 1 calc R . .
H13E H 1.3315 1.3237 0.6543 0.117 Uiso 1 1 calc R . .
H13F H 1.4541 1.3395 0.7659 0.117 Uiso 1 1 calc R . .
C140 C 1.1515(5) 1.3978(3) 0.7084(4) 0.0688(13) Uani 1 1 d . . .
H14A H 1.0795 1.3886 0.7372 0.103 Uiso 1 1 calc R . .
H14B H 1.1080 1.3638 0.6369 0.103 Uiso 1 1 calc R . .
H14C H 1.1934 1.4712 0.7113 0.103 Uiso 1 1 calc R . .
N2 N 0.6627(3) 0.8507(2) 0.5613(2) 0.0420(6) Uani 1 1 d . . .
C21 C 0.5382(4) 0.7992(3) 0.4695(3) 0.0525(9) Uani 1 1 d . . .
H21A H 0.4702 0.8390 0.4553 0.079 Uiso 1 1 calc R . .
H21B H 0.4952 0.7304 0.4803 0.079 Uiso 1 1 calc R . .
H21C H 0.5653 0.7934 0.4111 0.079 Uiso 1 1 calc R . .
C22 C 0.7279(4) 0.9529(3) 0.5461(3) 0.0548(9) Uani 1 1 d . . .
H22A H 0.7589 0.9471 0.4896 0.082 Uiso 1 1 calc R . .
H22B H 0.8094 0.9880 0.6091 0.082 Uiso 1 1 calc R . .
H22C H 0.6593 0.9924 0.5292 0.082 Uiso 1 1 calc R . .
N3 N 0.7074(3) 0.9156(2) 0.8024(2) 0.0459(7) Uani 1 1 d . . .
C31 C 0.7693(5) 0.9274(3) 0.9142(3) 0.0584(10) Uani 1 1 d . . .
H31A H 0.8209 0.9997 0.9425 0.088 Uiso 1 1 calc R . .
H31B H 0.8342 0.8853 0.9358 0.088 Uiso 1 1 calc R . .
H31C H 0.6943 0.9052 0.9394 0.088 Uiso 1 1 calc R . .
C32 C 0.6154(5) 0.9805(3) 0.7674(4) 0.0638(11) Uani 1 1 d . . .
H32A H 0.5387 0.9613 0.7914 0.096 Uiso 1 1 calc R . .
H32B H 0.5759 0.9715 0.6923 0.096 Uiso 1 1 calc R . .
H32C H 0.6695 1.0525 0.7951 0.096 Uiso 1 1 calc R . .
N4 N 0.5855(3) 0.6881(2) 0.6996(2) 0.0425(6) Uani 1 1 d . . .
C41 C 0.5502(4) 0.5968(3) 0.6265(3) 0.0514(9) Uani 1 1 d . . .
H41A H 0.5762 0.5413 0.6637 0.077 Uiso 1 1 calc R . .
H41B H 0.6018 0.6123 0.5820 0.077 Uiso 1 1 calc R . .
H41C H 0.4486 0.5754 0.5846 0.077 Uiso 1 1 calc R . .
C42 C 0.5151(4) 0.6669(3) 0.7697(4) 0.0544(10) Uani 1 1 d . . .
H42A H 0.4132 0.6393 0.7303 0.082 Uiso 1 1 calc R . .
H42B H 0.5348 0.7305 0.8146 0.082 Uiso 1 1 calc R . .
H42C H 0.5498 0.6164 0.8113 0.082 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'
Zr Zr -2.9673 0.5597 '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
N2 Zr1 N3 108.27(12) . . ?
N2 Zr1 N4 101.37(12) . . ?
N3 Zr1 N4 97.53(12) . . ?
N2 Zr1 N1 118.54(11) . . ?
N3 Zr1 N1 130.27(11) . . ?
N4 Zr1 N1 89.26(10) . . ?
N2 Zr1 C1 106.05(11) . . ?
N3 Zr1 C1 88.67(11) . . ?
N4 Zr1 C1 148.37(11) . . ?
N1 Zr1 C1 63.93(9) . . ?
N2 Zr1 P1 110.15(8) . . ?
N3 Zr1 P1 117.58(9) . . ?
N4 Zr1 P1 120.11(8) . . ?
N1 Zr1 P1 30.94(6) . . ?
C1 Zr1 P1 34.24(7) . . ?
C11 N1 P1 126.5(2) . . ?
C11 N1 Zr1 129.7(2) . . ?
P1 N1 Zr1 103.56(12) . . ?
C16 C11 C12 119.4(3) . . ?
C16 C11 N1 121.4(3) . . ?
C12 C11 N1 119.0(3) . . ?
C13 C12 C11 119.3(3) . . ?
C13 C12 C17 120.0(3) . . ?
C11 C12 C17 120.7(3) . . ?
C14 C13 C12 122.3(3) . . ?
C13 C14 C15 117.5(3) . . ?
C13 C14 C18 121.0(3) . . ?
C15 C14 C18 121.5(3) . . ?
C14 C15 C16 122.4(3) . . ?
C15 C16 C11 119.0(3) . . ?
C15 C16 C19 119.3(3) . . ?
C11 C16 C19 121.7(3) . . ?
N1 P1 C1 99.27(14) . . ?
N1 P1 C121 114.52(14) . . ?
C1 P1 C121 111.52(15) . . ?
N1 P1 C111 113.39(14) . . ?
C1 P1 C111 115.48(15) . . ?
C121 P1 C111 103.19(15) . . ?
N1 P1 Zr1 45.50(9) . . ?
C1 P1 Zr1 56.13(11) . . ?
C121 P1 Zr1 114.56(11) . . ?
C111 P1 Zr1 141.81(10) . . ?
C116 C111 C112 119.5(3) . . ?
C116 C111 P1 117.0(2) . . ?
C112 C111 P1 123.5(2) . . ?
C113 C112 C111 119.4(3) . . ?
C114 C113 C112 120.3(3) . . ?
C115 C114 C113 120.2(3) . . ?
C114 C115 C116 120.0(3) . . ?
C115 C116 C111 120.6(3) . . ?
C122 C121 C126 118.9(3) . . ?
C122 C121 P1 122.4(2) . . ?
C126 C121 P1 118.7(3) . . ?
C123 C122 C121 121.0(3) . . ?
C124 C123 C122 119.6(3) . . ?
C123 C124 C125 120.1(3) . . ?
C126 C125 C124 120.3(3) . . ?
C125 C126 C121 120.0(3) . . ?
C131 C1 P1 127.9(2) . . ?
C131 C1 Zr1 130.5(2) . . ?
P1 C1 Zr1 89.63(12) . . ?
C136 C131 C132 115.6(3) . . ?
C136 C131 C1 126.3(3) . . ?
C132 C131 C1 118.1(3) . . ?
C133 C132 C131 122.4(3) . . ?
C132 C133 C134 122.0(3) . . ?
C135 C134 C133 115.7(3) . . ?
C135 C134 C137 123.9(3) . . ?
C133 C134 C137 120.4(3) . . ?
C136 C135 C134 122.5(3) . . ?
C135 C136 C131 121.8(3) . . ?
C139 C137 C138 108.9(4) . . ?
C139 C137 C134 111.5(3) . . ?
C138 C137 C134 109.9(3) . . ?
C139 C137 C140 108.4(4) . . ?
C138 C137 C140 107.8(3) . . ?
C134 C137 C140 110.3(3) . . ?
C21 N2 C22 110.0(3) . . ?
C21 N2 Zr1 133.1(2) . . ?
C22 N2 Zr1 116.1(2) . . ?
C32 N3 C31 111.1(3) . . ?
C32 N3 Zr1 124.5(3) . . ?
C31 N3 Zr1 124.4(3) . . ?
C42 N4 C41 111.0(3) . . ?
C42 N4 Zr1 128.5(2) . . ?
C41 N4 Zr1 119.8(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
Zr1 N2 2.048(3) . ?
Zr1 N3 2.049(3) . ?
Zr1 N4 2.064(3) . ?
Zr1 N1 2.262(3) . ?
Zr1 C1 2.560(3) . ?
Zr1 P1 3.0832(9) . ?
N1 C11 1.436(4) . ?
N1 P1 1.631(3) . ?
C11 C16 1.406(5) . ?
C11 C12 1.409(4) . ?
C12 C13 1.389(5) . ?
C12 C17 1.507(5) . ?
C13 C14 1.388(5) . ?
C14 C15 1.390(5) . ?
C14 C18 1.515(5) . ?
C15 C16 1.393(4) . ?
C16 C19 1.513(5) . ?
P1 C1 1.735(3) . ?
P1 C121 1.811(3) . ?
P1 C111 1.817(3) . ?
C111 C116 1.394(4) . ?
C111 C112 1.397(4) . ?
C112 C113 1.392(5) . ?
C113 C114 1.389(5) . ?
C114 C115 1.378(5) . ?
C115 C116 1.380(5) . ?
C121 C122 1.390(5) . ?
C121 C126 1.401(5) . ?
C122 C123 1.385(5) . ?
C123 C124 1.380(5) . ?
C124 C125 1.394(5) . ?
C125 C126 1.378(5) . ?
C1 C131 1.487(4) . ?
C131 C136 1.397(5) . ?
C131 C132 1.403(4) . ?
C132 C133 1.380(4) . ?
C133 C134 1.400(5) . ?
C134 C135 1.391(5) . ?
C134 C137 1.533(4) . ?
C135 C136 1.388(4) . ?
C137 C139 1.523(5) . ?
C137 C138 1.528(5) . ?
C137 C140 1.535(5) . ?
N2 C21 1.456(5) . ?
N2 C22 1.457(5) . ?
N3 C32 1.450(5) . ?
N3 C31 1.459(5) . ?
N4 C42 1.453(5) . ?
N4 C41 1.455(5) . ?
