#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/34/7013444.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_7013444
loop_
_publ_author_name
'Hollink, Emily'
'Stewart, Jeffrey C.'
'Wei, Pingrong'
'Stephan, Douglas W.'
_publ_section_title
;
 Ti and Zr bidentate bis-phosphinimide complexes
;
_journal_issue                   20
_journal_name_full               'Dalton Transactions'
_journal_page_first              3968
_journal_paper_doi               10.1039/b308114a
_journal_year                    2003
_chemical_formula_sum            'C24 H46 N2 P2'
_chemical_formula_weight         424.57
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.388(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.457(8)
_cell_length_b                   13.908(8)
_cell_length_c                   14.713(8)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.0
_cell_volume                     2613(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0271
_diffrn_reflns_av_sigmaI/netI    0.0338
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10896
_diffrn_reflns_theta_full        23.17
_diffrn_reflns_theta_max         23.17
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    0.178
_exptl_absorpt_correction_T_max  0.488950
_exptl_absorpt_correction_T_min  0.321773
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_density_diffrn    1.079
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.357
_refine_diff_density_min         -0.245
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         3714
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0422
_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)+(0.0897P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1236
_refine_ls_wR_factor_ref         0.1333
_reflns_number_gt                2709
_reflns_number_total             3714
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b308114a.txt
_cod_data_source_block           m-C6H4(CH2(t-Bu2)PNH)2
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7013444
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
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.70529(5) 0.81918(5) -0.22319(5) 0.0429(2) Uani 1 1 d . . .
P2 P 0.77437(5) 0.97172(4) 0.20935(4) 0.0393(2) Uani 1 1 d . . .
N1 N 0.7683(2) 0.91622(18) -0.19604(17) 0.0644(7) Uani 1 1 d . . .
N2 N 0.80992(19) 0.86285(16) 0.22209(16) 0.0605(7) Uani 1 1 d . . .
C1 C 0.57446(19) 0.8256(2) -0.20723(18) 0.0481(7) Uani 1 1 d . . .
H1A H 0.5389 0.8815 -0.2420 0.058 Uiso 1 1 calc R . .
H1B H 0.5352 0.7695 -0.2380 0.058 Uiso 1 1 calc R . .
C2 C 0.56699(18) 0.83095(18) -0.10718(18) 0.0415(6) Uani 1 1 d . . .
C3 C 0.5100(2) 0.76182(19) -0.0759(2) 0.0499(7) Uani 1 1 d . . .
H3A H 0.4779 0.7116 -0.1162 0.060 Uiso 1 1 calc R . .
C4 C 0.5011(2) 0.7679(2) 0.0150(2) 0.0575(8) Uani 1 1 d . . .
H4A H 0.4627 0.7218 0.0353 0.069 Uiso 1 1 calc R . .
C5 C 0.5485(2) 0.8416(2) 0.0760(2) 0.0543(7) Uani 1 1 d . . .
H5A H 0.5434 0.8436 0.1376 0.065 Uiso 1 1 calc R . .
C6 C 0.60415(18) 0.91359(17) 0.04639(18) 0.0423(6) Uani 1 1 d . . .
C7 C 0.61193(19) 0.90639(18) -0.04570(18) 0.0430(6) Uani 1 1 d . . .
H7A H 0.6484 0.9536 -0.0668 0.052 Uiso 1 1 calc R . .
C8 C 0.6706(2) 0.7986(2) -0.35538(19) 0.0617(8) Uani 1 1 d . . .
C9 C 0.7692(3) 0.8100(3) -0.3862(2) 0.0920(12) Uani 1 1 d . . .
H9A H 0.7513 0.7999 -0.4540 0.138 Uiso 1 1 calc R . .
H9B H 0.8208 0.7637 -0.3530 0.138 Uiso 1 1 calc R . .
H9C H 0.7970 0.8737 -0.3707 0.138 Uiso 1 1 calc R . .
C10 C 0.5924(3) 0.8798(3) -0.4060(2) 0.0871(12) Uani 1 1 d . . .
H10A H 0.5731 0.8717 -0.4742 0.131 Uiso 1 1 calc R . .
H10B H 0.6252 0.9413 -0.3886 0.131 Uiso 1 1 calc R . .
H10C H 0.5309 0.8762 -0.3864 0.131 Uiso 1 1 calc R . .
C11 C 0.6202(3) 0.7004(3) -0.3883(2) 0.0882(11) Uani 1 1 d . . .
H11A H 0.6046 0.6947 -0.4564 0.132 Uiso 1 1 calc R . .
H11B H 0.5568 0.6948 -0.3720 0.132 Uiso 1 1 calc R . .
H11C H 0.6679 0.6503 -0.3570 0.132 Uiso 1 1 calc R . .
C12 C 0.7747(2) 0.7140(2) -0.1517(2) 0.0563(7) Uani 1 1 d . . .
C13 C 0.8208(3) 0.7494(2) -0.0477(2) 0.0760(10) Uani 1 1 d . . .
H13A H 0.8575 0.6976 -0.0080 0.114 Uiso 1 1 calc R . .
H13B H 0.7652 0.7712 -0.0250 0.114 Uiso 1 1 calc R . .
H13C H 0.8686 0.8014 -0.0452 0.114 Uiso 1 1 calc R . .
C14 C 0.7036(3) 0.6272(2) -0.1530(3) 0.0780(10) Uani 1 1 d . . .
H14A H 0.7444 0.5762 -0.1152 0.117 Uiso 1 1 calc R . .
H14B H 0.6726 0.6055 -0.2177 0.117 Uiso 1 1 calc R . .
H14C H 0.6494 0.6457 -0.1269 0.117 Uiso 1 1 calc R . .
C15 C 0.8678(3) 0.6821(3) -0.1856(3) 0.0808(10) Uani 1 1 d . . .
H15A H 0.9023 0.6280 -0.1483 0.121 Uiso 1 1 calc R . .
H15B H 0.9166 0.7343 -0.1776 0.121 Uiso 1 1 calc R . .
H15C H 0.8421 0.6643 -0.2520 0.121 Uiso 1 1 calc R . .
C16 C 0.6513(2) 0.99825(18) 0.11034(18) 0.0475(7) Uani 1 1 d . . .
H16A H 0.5998 1.0226 0.1381 0.057 Uiso 1 1 calc R . .
H16B H 0.6656 1.0490 0.0709 0.057 Uiso 1 1 calc R . .
C17 C 0.8739(2) 1.0512(2) 0.18136(19) 0.0528(7) Uani 1 1 d . . .
C18 C 0.8423(3) 1.1568(2) 0.1597(3) 0.0821(11) Uani 1 1 d . . .
H18A H 0.8977 1.1908 0.1456 0.123 Uiso 1 1 calc R . .
H18B H 0.8295 1.1854 0.2143 0.123 Uiso 1 1 calc R . .
H18C H 0.7798 1.1602 0.1055 0.123 Uiso 1 1 calc R . .
C19 C 0.8915(3) 1.0060(3) 0.0925(2) 0.0819(11) Uani 1 1 d . . .
H19A H 0.9416 1.0436 0.0737 0.123 Uiso 1 1 calc R . .
H19B H 0.8265 1.0044 0.0410 0.123 Uiso 1 1 calc R . .
H19C H 0.9176 0.9417 0.1071 0.123 Uiso 1 1 calc R . .
C20 C 0.9775(3) 1.0455(3) 0.2631(3) 0.1015(13) Uani 1 1 d . . .
H20A H 1.0284 1.0860 0.2488 0.152 Uiso 1 1 calc R . .
H20B H 1.0022 0.9803 0.2703 0.152 Uiso 1 1 calc R . .
H20C H 0.9670 1.0667 0.3215 0.152 Uiso 1 1 calc R . .
C21 C 0.7472(2) 1.00963(19) 0.32105(19) 0.0513(7) Uani 1 1 d . . .
C22 C 0.6514(3) 0.9523(2) 0.3264(3) 0.0849(11) Uani 1 1 d . . .
H22A H 0.6352 0.9702 0.3831 0.127 Uiso 1 1 calc R . .
H22B H 0.6667 0.8847 0.3284 0.127 Uiso 1 1 calc R . .
H22C H 0.5925 0.9661 0.2710 0.127 Uiso 1 1 calc R . .
C23 C 0.7227(3) 1.1174(2) 0.3233(2) 0.0660(9) Uani 1 1 d . . .
H23A H 0.7097 1.1324 0.3822 0.099 Uiso 1 1 calc R . .
H23B H 0.6619 1.1328 0.2703 0.099 Uiso 1 1 calc R . .
H23C H 0.7813 1.1542 0.3189 0.099 Uiso 1 1 calc R . .
C24 C 0.8398(3) 0.9833(3) 0.4103(2) 0.0934(12) Uani 1 1 d . . .
H24A H 0.8247 1.0035 0.4669 0.140 Uiso 1 1 calc R . .
H24B H 0.9020 1.0151 0.4072 0.140 Uiso 1 1 calc R . .
H24C H 0.8505 0.9150 0.4123 0.140 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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 P1 C1 112.60(13) . . ?
N1 P1 C12 113.14(14) . . ?
C1 P1 C12 107.02(13) . . ?
N1 P1 C8 109.40(13) . . ?
C1 P1 C8 101.74(12) . . ?
C12 P1 C8 112.40(14) . . ?
N2 P2 C21 107.57(13) . . ?
N2 P2 C17 112.30(14) . . ?
C21 P2 C17 112.17(13) . . ?
N2 P2 C16 116.29(12) . . ?
C21 P2 C16 105.02(13) . . ?
C17 P2 C16 103.34(13) . . ?
C2 C1 P1 119.02(17) . . ?
C7 C2 C3 118.4(2) . . ?
C7 C2 C1 121.5(2) . . ?
C3 C2 C1 120.0(2) . . ?
C4 C3 C2 120.1(2) . . ?
C3 C4 C5 120.8(3) . . ?
C6 C5 C4 120.8(3) . . ?
C5 C6 C7 117.6(2) . . ?
C5 C6 C16 121.5(2) . . ?
C7 C6 C16 120.9(2) . . ?
C2 C7 C6 122.3(2) . . ?
C11 C8 C9 109.6(3) . . ?
C11 C8 C10 109.2(3) . . ?
C9 C8 C10 107.3(3) . . ?
C11 C8 P1 113.9(2) . . ?
C9 C8 P1 109.5(2) . . ?
C10 C8 P1 107.1(2) . . ?
C14 C12 C15 109.5(3) . . ?
C14 C12 C13 108.5(3) . . ?
C15 C12 C13 107.4(3) . . ?
C14 C12 P1 114.1(2) . . ?
C15 C12 P1 110.7(2) . . ?
C13 C12 P1 106.4(2) . . ?
C6 C16 P2 115.21(17) . . ?
C19 C17 C18 108.8(3) . . ?
C19 C17 C20 107.5(3) . . ?
C18 C17 C20 109.7(3) . . ?
C19 C17 P2 105.0(2) . . ?
C18 C17 P2 116.0(2) . . ?
C20 C17 P2 109.5(2) . . ?
C23 C21 C24 109.5(3) . . ?
C23 C21 C22 108.4(3) . . ?
C24 C21 C22 107.4(3) . . ?
C23 C21 P2 113.37(19) . . ?
C24 C21 P2 110.6(2) . . ?
C22 C21 P2 107.3(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
P1 N1 1.577(2) . ?
P1 C1 1.850(3) . ?
P1 C12 1.870(3) . ?
P1 C8 1.873(3) . ?
P2 N2 1.581(2) . ?
P2 C21 1.869(3) . ?
P2 C17 1.879(3) . ?
P2 C16 1.865(3) . ?
C1 C2 1.509(4) . ?
C2 C7 1.393(3) . ?
C2 C3 1.396(4) . ?
C3 C4 1.382(4) . ?
C4 C5 1.380(4) . ?
C5 C6 1.399(4) . ?
C6 C7 1.395(3) . ?
C6 C16 1.516(3) . ?
C8 C11 1.533(4) . ?
C8 C9 1.540(4) . ?
C8 C10 1.563(5) . ?
C12 C14 1.537(4) . ?
C12 C15 1.552(4) . ?
C12 C13 1.539(4) . ?
C17 C19 1.536(4) . ?
C17 C18 1.534(4) . ?
C17 C20 1.530(4) . ?
C21 C23 1.537(4) . ?
C21 C24 1.543(4) . ?
C21 C22 1.539(4) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 4418697
