#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/19/7011952.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_7011952
loop_
_publ_author_name
'Baldamus, Jens'
'Berghof, Christiane'
'Cole, Marcus L.'
'Evans, David J.'
'Hey-Hawkins, Evamarie'
'Junk, Peter C.'
_publ_section_title
;
 N,N???-Di(tolyl)formamidinate complexes of potassium: studies of
 ancillary donor imposed molecular and supramolecular structure
;
_journal_issue                   22
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4185
_journal_paper_doi               10.1039/b206165a
_journal_year                    2002
_chemical_formula_moiety         'C19 H25 K N2 O2'
_chemical_formula_sum            'C19 H25 K N2 O2'
_chemical_formula_weight         352.51
_chemical_name_common            '[{K(FTolP)(DME)}n]'
_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                107.764(3)
_cell_angle_beta                 90.529(3)
_cell_angle_gamma                108.107(3)
_cell_formula_units_Z            2
_cell_length_a                   7.7331(11)
_cell_length_b                   10.4662(14)
_cell_length_c                   13.3689(19)
_cell_measurement_temperature    123(2)
_cell_volume                     972.9(2)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'Nonius Collect'
_computing_data_reduction        'X -Seed'
_computing_molecular_graphics    'X-Seed / POV-Ray'
_computing_publication_material  'Microsoft Office 2000'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'Single Crystal'
_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  0.0546
_diffrn_reflns_av_sigmaI/netI    0.0846
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6518
_diffrn_reflns_theta_full        27.98
_diffrn_reflns_theta_max         27.98
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    0.285
_exptl_absorpt_correction_T_max  0.9451
_exptl_absorpt_correction_T_min  0.9193
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'performed as part of the DENZO-SMN package'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             376
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.420
_refine_diff_density_min         -0.344
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.938
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         4496
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.938
_refine_ls_R_factor_all          0.1059
_refine_ls_R_factor_gt           0.0632
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0928P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1457
_refine_ls_wR_factor_ref         0.1744
_reflns_number_gt                2677
_reflns_number_total             4496
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b206165a.txt
_cod_data_source_block           Compound_3
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7011952
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
K1 K 0.29724(8) 0.02898(6) 0.52961(5) 0.0381(2) Uani 1 1 d . . .
O1 O 0.1873(3) 0.1713(2) 0.71466(19) 0.0509(6) Uani 1 1 d . . .
N1 N 0.3338(3) -0.2524(2) 0.40793(19) 0.0354(5) Uani 1 1 d . . .
C1 C 0.2273(4) -0.3697(3) 0.3244(2) 0.0346(6) Uani 1 1 d . . .
O2 O -0.0525(3) -0.0962(2) 0.58753(16) 0.0402(5) Uani 1 1 d . . .
N2 N 0.4400(3) -0.1613(2) 0.58396(19) 0.0341(5) Uani 1 1 d . . .
C2 C 0.0844(4) -0.4841(3) 0.3363(3) 0.0373(7) Uani 1 1 d . . .
C3 C -0.0188(4) -0.5957(3) 0.2498(3) 0.0422(7) Uani 1 1 d . . .
C4 C 0.0120(4) -0.5987(3) 0.1473(3) 0.0434(7) Uani 1 1 d . . .
C5 C 0.1503(4) -0.4853(3) 0.1348(3) 0.0433(7) Uani 1 1 d . . .
C6 C 0.2538(4) -0.3728(3) 0.2204(3) 0.0397(7) Uani 1 1 d . . .
C7 C -0.1029(6) -0.7218(5) 0.0551(4) 0.0634(11) Uani 1 1 d . . .
C8 C 0.4862(4) -0.1822(3) 0.6776(2) 0.0330(6) Uani 1 1 d . . .
C9 C 0.5092(4) -0.3062(3) 0.6876(3) 0.0364(7) Uani 1 1 d . . .
C10 C 0.5616(4) -0.3117(3) 0.7847(3) 0.0425(7) Uani 1 1 d . . .
C11 C 0.5969(4) -0.1968(4) 0.8771(3) 0.0445(7) Uani 1 1 d . . .
C12 C 0.5768(4) -0.0731(3) 0.8668(3) 0.0443(7) Uani 1 1 d . . .
C13 C 0.5224(4) -0.0667(3) 0.7708(2) 0.0399(7) Uani 1 1 d . . .
C14 C 0.6513(8) -0.2055(7) 0.9824(4) 0.0681(12) Uani 1 1 d . . .
C15 C 0.3616(4) -0.2698(3) 0.4993(2) 0.0336(6) Uani 1 1 d . . .
C16 C 0.0235(5) 0.0982(4) 0.7479(3) 0.0488(8) Uani 1 1 d . . .
C17 C -0.0145(5) -0.0587(3) 0.6993(3) 0.0436(7) Uani 1 1 d . . .
C18 C 0.2416(6) 0.3212(4) 0.7649(4) 0.0616(10) Uani 1 1 d . . .
C19 C -0.0923(6) -0.2447(4) 0.5359(3) 0.0525(9) Uani 1 1 d . . .
H19B H -0.099(6) -0.269(4) 0.454(4) 0.087(14) Uiso 1 1 d . . .
H19C H -0.211(5) -0.299(4) 0.553(3) 0.071(12) Uiso 1 1 d . . .
H19A H 0.004(6) -0.278(4) 0.551(3) 0.077(13) Uiso 1 1 d . . .
H12 H 0.601(4) 0.012(3) 0.930(3) 0.042(8) Uiso 1 1 d . . .
H5 H 0.169(4) -0.485(3) 0.063(2) 0.032(7) Uiso 1 1 d . . .
H6 H 0.342(4) -0.298(3) 0.208(2) 0.029(7) Uiso 1 1 d . . .
H15 H 0.324(4) -0.364(3) 0.500(2) 0.032(7) Uiso 1 1 d . . .
H18B H 0.291(5) 0.344(4) 0.837(4) 0.078(13) Uiso 1 1 d . . .
H17A H -0.122(5) -0.110(3) 0.730(3) 0.053(9) Uiso 1 1 d . . .
H7A H -0.239(7) -0.732(5) 0.054(4) 0.104(16) Uiso 1 1 d . . .
H7B H -0.112(8) -0.821(7) 0.050(5) 0.15(2) Uiso 1 1 d . . .
H16B H -0.075(4) 0.121(3) 0.727(2) 0.041(9) Uiso 1 1 d . . .
H9 H 0.484(4) -0.394(3) 0.621(3) 0.043(8) Uiso 1 1 d . . .
H7C H -0.069(7) -0.710(5) -0.008(4) 0.105(19) Uiso 1 1 d . . .
H10 H 0.580(5) -0.388(4) 0.788(3) 0.066(11) Uiso 1 1 d . . .
H16A H 0.038(5) 0.132(4) 0.830(3) 0.065(11) Uiso 1 1 d . . .
H13 H 0.511(4) 0.016(4) 0.767(3) 0.050(9) Uiso 1 1 d . . .
H17B H 0.101(4) -0.082(3) 0.709(2) 0.036(8) Uiso 1 1 d . . .
H2 H 0.048(4) -0.488(3) 0.404(3) 0.039(8) Uiso 1 1 d . . .
H14B H 0.742(11) -0.134(8) 1.023(6) 0.18(3) Uiso 1 1 d . . .
H14C H 0.725(8) -0.257(6) 0.978(4) 0.12(2) Uiso 1 1 d . . .
H14A H 0.567(7) -0.220(5) 1.025(4) 0.094(17) Uiso 1 1 d . . .
H3 H -0.127(5) -0.674(4) 0.261(3) 0.058(10) Uiso 1 1 d . . .
H18A H 0.147(6) 0.358(5) 0.753(3) 0.088(14) Uiso 1 1 d . . .
H18C H 0.356(5) 0.357(4) 0.735(3) 0.056(11) Uiso 1 1 d . . .
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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
O1 K1 N2 124.48(7) . 2_656 ?
O1 K1 N2 104.80(7) . . ?
N2 K1 N2 105.05(6) 2_656 . ?
O1 K1 O2 89.58(7) . 2_556 ?
N2 K1 O2 83.76(7) 2_656 2_556 ?
N2 K1 O2 153.42(7) . 2_556 ?
O1 K1 O2 60.46(6) . . ?
N2 K1 O2 158.99(7) 2_656 . ?
N2 K1 O2 91.90(6) . . ?
O2 K1 O2 75.67(6) 2_556 . ?
O1 K1 N1 88.50(7) . 2_656 ?
N2 K1 N1 46.28(7) 2_656 2_656 ?
N2 K1 N1 89.83(7) . 2_656 ?
O2 K1 N1 113.16(6) 2_556 2_656 ?
O2 K1 N1 148.27(7) . 2_656 ?
O1 K1 N1 142.94(7) . . ?
N2 K1 N1 89.57(7) 2_656 . ?
N2 K1 N1 46.15(7) . . ?
O2 K1 N1 110.27(7) 2_556 . ?
O2 K1 N1 93.52(6) . . ?
N1 K1 N1 110.10(5) 2_656 . ?
O1 K1 C15 101.86(7) . 2_656 ?
N2 K1 C15 24.51(7) 2_656 2_656 ?
N2 K1 C15 105.85(7) . 2_656 ?
O2 K1 C15 92.52(7) 2_556 2_656 ?
O2 K1 C15 158.15(7) . 2_656 ?
N1 K1 C15 24.52(7) 2_656 2_656 ?
N1 K1 C15 107.92(7) . 2_656 ?
O1 K1 C15 121.16(7) . . ?
N2 K1 C15 104.05(7) 2_656 . ?
N2 K1 C15 23.84(7) . . ?
O2 K1 C15 130.10(7) 2_556 . ?
O2 K1 C15 86.40(6) . . ?
N1 K1 C15 106.45(7) 2_656 . ?
N1 K1 C15 24.04(7) . . ?
C15 K1 C15 114.93(6) 2_656 . ?
O1 K1 K1 132.47(6) . 2_656 ?
N2 K1 K1 52.53(5) 2_656 2_656 ?
N2 K1 K1 52.52(5) . 2_656 ?
O2 K1 K1 130.21(5) 2_556 2_656 ?
O2 K1 K1 142.59(5) . 2_656 ?
N1 K1 K1 55.23(5) 2_656 2_656 ?
N1 K1 K1 54.87(5) . 2_656 ?
C15 K1 K1 58.45(5) 2_656 2_656 ?
C15 K1 K1 56.48(5) . 2_656 ?
O1 K1 C19 74.11(9) . 2_556 ?
N2 K1 C19 78.67(8) 2_656 2_556 ?
N2 K1 C19 175.84(8) . 2_556 ?
O2 K1 C19 23.89(8) 2_556 2_556 ?
O2 K1 C19 84.07(8) . 2_556 ?
N1 K1 C19 94.14(8) 2_656 2_556 ?
N1 K1 C19 132.89(8) . 2_556 ?
C15 K1 C19 78.31(8) 2_656 2_556 ?
C15 K1 C19 153.98(9) . 2_556 ?
K1 K1 C19 131.16(7) 2_656 2_556 ?
O1 K1 C17 43.35(7) . . ?
N2 K1 C17 167.68(7) 2_656 . ?
N2 K1 C17 82.80(7) . . ?
O2 K1 C17 93.36(7) 2_556 . ?
O2 K1 C17 23.98(7) . . ?
N1 K1 C17 125.72(7) 2_656 . ?
N1 K1 C17 102.64(7) . . ?
C15 K1 C17 144.58(8) 2_656 . ?
C15 K1 C17 86.99(8) . . ?
K1 K1 C17 134.41(6) 2_656 . ?
C19 K1 C17 93.86(9) 2_556 . ?
C16 O1 C18 112.3(3) . . ?
C16 O1 K1 117.88(18) . . ?
C18 O1 K1 126.9(2) . . ?
C15 N1 C1 118.5(2) . . ?
C15 N1 K1 84.84(16) . 2_656 ?
C1 N1 K1 142.74(18) . 2_656 ?
C15 N1 K1 87.54(16) . . ?
C1 N1 K1 134.40(17) . . ?
K1 N1 K1 69.90(5) 2_656 . ?
N1 C1 C6 119.2(2) . . ?
N1 C1 C2 124.6(3) . . ?
C6 C1 C2 116.1(3) . . ?
C19 O2 C17 111.8(3) . . ?
C19 O2 K1 102.8(2) . 2_556 ?
C17 O2 K1 129.38(18) . 2_556 ?
C19 O2 K1 103.98(19) . . ?
C17 O2 K1 101.93(17) . . ?
K1 O2 K1 104.33(6) 2_556 . ?
C15 N2 C8 120.6(2) . . ?
C15 N2 K1 92.21(17) . 2_656 ?
C8 N2 K1 122.96(16) . 2_656 ?
C15 N2 K1 95.68(17) . . ?
C8 N2 K1 135.95(17) . . ?
K1 N2 K1 74.95(6) 2_656 . ?
C3 C2 C1 121.6(3) . . ?
C4 C3 C2 121.5(3) . . ?
C5 C4 C3 117.2(3) . . ?
C5 C4 C7 122.6(3) . . ?
C3 C4 C7 120.1(3) . . ?
C6 C5 C4 121.9(3) . . ?
C5 C6 C1 121.6(3) . . ?
N2 C8 C13 117.3(3) . . ?
N2 C8 C9 126.6(3) . . ?
C13 C8 C9 116.0(3) . . ?
C10 C9 C8 121.0(3) . . ?
C9 C10 C11 122.7(3) . . ?
C10 C11 C12 116.2(3) . . ?
C10 C11 C14 121.9(3) . . ?
C12 C11 C14 121.9(3) . . ?
C13 C12 C11 121.6(3) . . ?
C12 C13 C8 122.4(3) . . ?
N2 C15 N1 121.3(2) . . ?
N2 C15 K1 63.28(14) . 2_656 ?
N1 C15 K1 70.64(15) . 2_656 ?
N2 C15 K1 60.49(14) . . ?
N1 C15 K1 68.42(15) . . ?
K1 C15 K1 65.07(6) 2_656 . ?
O1 C16 C17 108.9(3) . . ?
O2 C17 C16 108.6(3) . . ?
O2 C17 K1 54.09(14) . . ?
C16 C17 K1 85.83(18) . . ?
O2 C19 K1 53.35(16) . 2_556 ?
O2 C19 K1 52.56(15) . . ?
K1 C19 K1 80.77(8) 2_556 . ?
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
K1 O1 2.764(2) . ?
K1 N2 2.818(2) 2_656 ?
K1 N2 2.819(2) . ?
K1 O2 2.824(2) 2_556 ?
K1 O2 2.843(2) . ?
K1 N1 2.987(2) 2_656 ?
K1 N1 3.000(2) . ?
K1 C15 3.153(3) 2_656 ?
K1 C15 3.223(3) . ?
K1 K1 3.4299(13) 2_656 ?
K1 C19 3.433(4) 2_556 ?
K1 C17 3.435(3) . ?
O1 C16 1.415(4) . ?
O1 C18 1.426(4) . ?
N1 C15 1.314(4) . ?
N1 C1 1.397(4) . ?
N1 K1 2.987(2) 2_656 ?
C1 C6 1.399(4) . ?
C1 C2 1.407(4) . ?
O2 C19 1.425(4) . ?
O2 C17 1.427(4) . ?
O2 K1 2.824(2) 2_556 ?
N2 C15 1.309(4) . ?
N2 C8 1.396(4) . ?
N2 K1 2.818(2) 2_656 ?
C2 C3 1.385(4) . ?
C3 C4 1.385(5) . ?
C4 C5 1.385(4) . ?
C4 C7 1.506(5) . ?
C5 C6 1.382(4) . ?
C8 C13 1.399(4) . ?
C8 C9 1.409(4) . ?
C9 C10 1.379(4) . ?
C10 C11 1.390(5) . ?
C11 C12 1.397(4) . ?
C11 C14 1.503(5) . ?
C12 C13 1.374(4) . ?
C15 K1 3.153(3) 2_656 ?
C16 C17 1.500(5) . ?
C19 K1 3.433(4) 2_556 ?
