#------------------------------------------------------------------------------
#$Date: 2016-03-21 15:23:04 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178745 $
#$URL: svn://www.crystallography.net/cod/cif/4/08/56/4085657.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_4085657
loop_
_publ_author_name
'Taylor, Morgan J.'
'Coakley, Emma J.'
'Coles, Martyn P.'
'Cox, Hazel'
'Fulton, J. Robin'
_publ_section_title
;
 β-Diketiminato Organolead Complexes: Structures,207Pb NMR, and Hammett
 Correlations
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2515
_journal_paper_doi               10.1021/om501223a
_journal_volume                  34
_journal_year                    2015
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C36 H48 N2 Pb1'
_chemical_formula_sum            'C36 H48 N2 Pb'
_chemical_formula_weight         715.95
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      62
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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             2009-05-28T11:09:59-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.2236(2)
_cell_length_b                   20.5353(2)
_cell_length_c                   9.9380(1)
_cell_measurement_reflns_used    35389
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.395
_cell_measurement_wavelength     0.71073
_cell_volume                     3310.91(6)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_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_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.258745E-1
_diffrn_orient_matrix_UB_12      -0.57953E-1
_diffrn_orient_matrix_UB_13      0.108769E-1
_diffrn_orient_matrix_UB_21      -0.24711E-2
_diffrn_orient_matrix_UB_22      0.138502E-1
_diffrn_orient_matrix_UB_23      0.474363E-1
_diffrn_orient_matrix_UB_31      -0.972089E-1
_diffrn_orient_matrix_UB_32      -0.157777E-1
_diffrn_orient_matrix_UB_33      0.16893E-2
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0783
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            51139
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.61
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    5.12
_exptl_absorpt_correction_T_max  0.4376
_exptl_absorpt_correction_T_min  0.3359
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            oRANGE
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bLOCK
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         3.072
_refine_diff_density_min         -1.485
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         3882
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0262
_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)+(0.0248P)²+6.4826P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0619
_refine_ls_wR_factor_ref         0.0639
_reflns_number_gt                3523
_reflns_number_total             3882
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om501223a_si_002.cif
_cod_data_source_block           Compound8-may909b
_cod_depositor_comments
'Adding full bibliography for 4085653--4085657.cif.'
_cod_database_code               4085657
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, 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
Pb Pb 0.140169(9) 0.25 0.532977(14) 0.02126(6) Uani 1 2 d S
N1 N 0.17302(15) 0.32281(11) 0.7033(2) 0.0195(5) Uani 1 1 d .
C1 C 0.24181(19) 0.31190(14) 0.7723(3) 0.0212(6) Uani 1 1 d .
C2 C 0.2774(3) 0.25 0.7891(4) 0.0226(9) Uani 1 2 d S
H2 H 0.3337 0.25 0.8157 0.027 Uiso 1 2 calc SR
C3 C 0.2857(2) 0.36747(16) 0.8411(4) 0.0341(8) Uani 1 1 d .
H3A H 0.2637 0.4089 0.8081 0.051 Uiso 1 1 calc R
H3B H 0.3448 0.3651 0.8213 0.051 Uiso 1 1 calc R
H3C H 0.2772 0.3645 0.9385 0.051 Uiso 1 1 calc R
C4 C 0.13290(18) 0.38500(15) 0.7051(3) 0.0232(6) Uani 1 1 d .
C5 C 0.0707(2) 0.39680(16) 0.8012(3) 0.0285(7) Uani 1 1 d .
C6 C 0.0293(2) 0.45598(18) 0.7961(4) 0.0374(8) Uani 1 1 d .
H6 H -0.0122 0.465 0.8609 0.045 Uiso 1 1 calc R
C7 C 0.0471(3) 0.50191(19) 0.6990(4) 0.0458(10) Uani 1 1 d .
H7 H 0.0177 0.5419 0.697 0.055 Uiso 1 1 calc R
C8 C 0.1073(3) 0.48974(18) 0.6055(4) 0.0402(9) Uani 1 1 d .
H8 H 0.1191 0.5216 0.539 0.048 Uiso 1 1 calc R
C9 C 0.1516(2) 0.43140(16) 0.6061(4) 0.0298(7) Uani 1 1 d .
C10 C 0.0497(2) 0.34767(17) 0.9097(4) 0.0346(8) Uani 1 1 d .
H10 H 0.0716 0.3045 0.8796 0.041 Uiso 1 1 calc R
C11 C 0.0911(4) 0.3639(3) 1.0429(5) 0.0714(16) Uani 1 1 d .
H11A H 0.0764 0.331 1.1101 0.107 Uiso 1 1 calc R
H11B H 0.0726 0.4068 1.0737 0.107 Uiso 1 1 calc R
H11C H 0.1511 0.3644 1.0308 0.107 Uiso 1 1 calc R
C12 C -0.0424(3) 0.3397(3) 0.9328(5) 0.0627(13) Uani 1 1 d .
H12A H -0.0517 0.3073 1.0036 0.094 Uiso 1 1 calc R
H12B H -0.0688 0.3252 0.8493 0.094 Uiso 1 1 calc R
H12C H -0.066 0.3816 0.9605 0.094 Uiso 1 1 calc R
C13 C 0.2183(2) 0.42036(17) 0.5003(3) 0.0319(7) Uani 1 1 d .
H13 H 0.2433 0.3766 0.517 0.038 Uiso 1 1 calc R
C14 C 0.1824(3) 0.4203(2) 0.3587(4) 0.0491(10) Uani 1 1 d .
H14A H 0.2266 0.413 0.2932 0.074 Uiso 1 1 calc R
H14B H 0.1561 0.4624 0.3408 0.074 Uiso 1 1 calc R
H14C H 0.1413 0.3856 0.3509 0.074 Uiso 1 1 calc R
C15 C 0.2869(3) 0.47166(19) 0.5125(5) 0.0458(10) Uani 1 1 d .
H15A H 0.3096 0.4709 0.6039 0.069 Uiso 1 1 calc R
H15B H 0.2642 0.5149 0.4937 0.069 Uiso 1 1 calc R
H15C H 0.3307 0.4619 0.4477 0.069 Uiso 1 1 calc R
C16 C 0.0012(3) 0.25 0.5855(5) 0.0366(11) Uani 1 2 d S
H16A H -0.0123 0.2109 0.6396 0.044 Uiso 0.5 1 calc PR
H16B H -0.0123 0.2891 0.6396 0.044 Uiso 0.5 1 calc PR
C17 C -0.0484(2) 0.25 0.4580(3) 0.0266(9) Uiso 1 2 d SG
C18 C -0.0655(3) 0.31248(4) 0.4120(4) 0.0360(17) Uiso 0.5 1 d PG
H18 H -0.0439 0.3492 0.4582 0.043 Uiso 0.5 1 calc PR
C19 C -0.1142(3) 0.32123(12) 0.2983(5) 0.0376(16) Uiso 0.5 1 d PG
H19 H -0.1259 0.3639 0.2669 0.045 Uiso 0.5 1 calc PR
C20 C -0.1458(2) 0.26751(18) 0.2307(4) 0.0354(17) Uiso 0.5 1 d PG
H20 H -0.179 0.2735 0.153 0.042 Uiso 0.5 1 calc PR
C21 C -0.1287(3) 0.20502(14) 0.2766(4) 0.0374(17) Uiso 0.5 1 d PG
H21 H -0.1502 0.1683 0.2304 0.045 Uiso 0.5 1 calc PR
C22 C -0.0800(3) 0.19627(5) 0.3903(4) 0.0337(16) Uiso 0.5 1 d PG
H22 H -0.0683 0.1536 0.4217 0.04 Uiso 0.5 1 calc PR
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 0 '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'
Pb Pb -3.3944 10.1111 '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
C16 Pb N1 93.38(11) . .
C16 Pb N1 93.38(11) . 8_565
N1 Pb N1 80.22(12) . 8_565
C1 N1 C4 121.7(2) . .
C1 N1 Pb 117.42(19) . .
C4 N1 Pb 118.61(18) . .
N1 C1 C2 124.0(3) . .
N1 C1 C3 120.2(3) . .
C2 C1 C3 115.8(3) . .
C1 C2 C1 129.4(4) 8_565 .
C1 C2 H2 115.3 8_565 .
C1 C2 H2 115.3 . .
C1 C3 H3A 109.5 . .
C1 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
C1 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
C9 C4 C5 120.9(3) . .
C9 C4 N1 119.9(3) . .
C5 C4 N1 119.1(3) . .
C6 C5 C4 118.1(3) . .
C6 C5 C10 120.0(3) . .
C4 C5 C10 121.9(3) . .
C7 C6 C5 121.5(3) . .
C7 C6 H6 119.3 . .
C5 C6 H6 119.3 . .
C8 C7 C6 119.9(3) . .
C8 C7 H7 120 . .
C6 C7 H7 120 . .
C7 C8 C9 121.3(4) . .
C7 C8 H8 119.3 . .
C9 C8 H8 119.3 . .
C8 C9 C4 118.3(3) . .
C8 C9 C13 119.3(3) . .
C4 C9 C13 122.4(3) . .
C5 C10 C12 113.6(3) . .
C5 C10 C11 112.0(3) . .
C12 C10 C11 109.0(4) . .
C5 C10 H10 107.3 . .
C12 C10 H10 107.3 . .
C11 C10 H10 107.3 . .
C10 C11 H11A 109.5 . .
C10 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
C10 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
C10 C12 H12A 109.5 . .
C10 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C10 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
C14 C13 C9 111.4(3) . .
C14 C13 C15 110.5(3) . .
C9 C13 C15 110.9(3) . .
C14 C13 H13 107.9 . .
C9 C13 H13 107.9 . .
C15 C13 H13 107.9 . .
C13 C14 H14A 109.5 . .
C13 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C13 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
C13 C15 H15A 109.5 . .
C13 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
C13 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
C17 C16 Pb 109.4(3) . .
C17 C16 H16A 109.8 . .
Pb C16 H16A 109.8 . .
C17 C16 H16B 109.8 . .
Pb C16 H16B 109.8 . .
H16A C16 H16B 108.3 . .
C18 C17 C18 134.8 8_565 .
C18 C17 C22 15.1 8_565 .
C18 C17 C22 120 . .
C18 C17 C22 120 8_565 8_565
C18 C17 C22 15.13(6) . 8_565
C22 C17 C22 105.07(6) . 8_565
C18 C17 C16 112.62(5) 8_565 .
C18 C17 C16 112.62(8) . .
C22 C17 C16 127.30(8) . .
C22 C17 C16 127.3 8_565 .
C17 C18 C19 120 . .
C17 C18 H18 120 . .
C19 C18 H18 120 . .
C20 C19 C18 120 . .
C20 C19 H19 120 . .
C18 C19 H19 120 . .
C21 C20 C19 120 . .
C21 C20 H20 120 . .
C19 C20 H20 120 . .
C20 C21 C22 120 . .
C20 C21 H21 120 . .
C22 C21 H21 120 . .
C21 C22 C17 120 . .
C21 C22 H22 120 . .
C17 C22 H22 120 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb C16 2.314(5) .
Pb N1 2.321(2) .
Pb N1 2.321(2) 8_565
N1 C1 1.329(4) .
N1 C4 1.433(4) .
C1 C2 1.406(3) .
C1 C3 1.509(4) .
C2 C1 1.406(3) 8_565
C2 H2 0.95 .
C3 H3A 0.98 .
C3 H3B 0.98 .
C3 H3C 0.98 .
C4 C9 1.403(5) .
C4 C5 1.410(5) .
C5 C6 1.390(5) .
C5 C10 1.515(5) .
C6 C7 1.380(6) .
C6 H6 0.95 .
C7 C8 1.371(6) .
C7 H7 0.95 .
C8 C9 1.397(5) .
C8 H8 0.95 .
C9 C13 1.525(5) .
C10 C12 1.521(6) .
C10 C11 1.522(6) .
C10 H10 1 .
C11 H11A 0.98 .
C11 H11B 0.98 .
C11 H11C 0.98 .
C12 H12A 0.98 .
C12 H12B 0.98 .
C12 H12C 0.98 .
C13 C14 1.524(5) .
C13 C15 1.538(5) .
C13 H13 1 .
C14 H14A 0.98 .
C14 H14B 0.98 .
C14 H14C 0.98 .
C15 H15A 0.98 .
C15 H15B 0.98 .
C15 H15C 0.98 .
C16 C17 1.502(6) .
C16 H16A 0.99 .
C16 H16B 0.99 .
C17 C18 1.3900(13) 8_565
C17 C18 1.39 .
C17 C22 1.39 .
C17 C22 1.3900(18) 8_565
C18 C19 1.39 .
C18 H18 0.95 .
C19 C20 1.39 .
C19 H19 0.95 .
C20 C21 1.39 .
C20 H20 0.95 .
C21 C22 1.39 .
C21 H21 0.95 .
C22 H22 0.95 .
