#------------------------------------------------------------------------------
#$Date: 2016-03-23 14:43:16 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179303 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/00/4320049.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_4320049
loop_
_publ_author_name
'Bin Du'
'Edward A. Meyers'
'Sheldon G. Shore'
_publ_section_title
;
 Syntheses and Structural Characterizations of Sheet- and Column-like
 Lanthanide-Transition Metal Arrays: The Effect of Hydrogen Bonding on the
 Structure When K+ Is Replaced by [NH4]+
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4353
_journal_page_last               4360
_journal_paper_doi               10.1021/ic0014787
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C20 H32 N13 O4 Pt2 Yb'
_chemical_formula_weight         1081.81
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 94.506(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            5
_cell_length_a                   9.0321(10)
_cell_length_b                   29.0623(10)
_cell_length_c                   15.3163(10)
_cell_measurement_temperature    213(2)
_cell_volume                     4008.0(5)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_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  0.0702
_diffrn_reflns_av_sigmaI/netI    0.1757
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -3
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7649
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.26
_exptl_absorpt_coefficient_mu    11.644
_exptl_absorpt_correction_T_max  0.1588
_exptl_absorpt_correction_T_min  0.0714
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    2.241
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2505
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         2.841
_refine_diff_density_min         -4.048
_refine_diff_density_rms         0.454
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         7032
_refine_ls_number_restraints     243
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.2156
_refine_ls_R_factor_gt           0.0852
_refine_ls_shift/su_max          2.928
_refine_ls_shift/su_mean         0.067
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1464P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2103
_refine_ls_wR_factor_ref         0.2637
_reflns_number_gt                3293
_reflns_number_total             7032
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0014787_3.cif
_cod_data_source_block           bd04
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4320049
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Yb Yb 0.33713(15) 0.46990(5) 1.22770(9) 0.0481(5) Uani 1 1 d . . .
Pt1 Pt -0.13862(12) 0.39880(4) 1.37364(7) 0.0327(3) Uani 1 1 d . A .
Pt2 Pt 0.58772(14) 0.61856(4) 1.07884(7) 0.0414(4) Uani 1 1 d . A .
N1 N 0.092(4) 0.4531(13) 1.2682(17) 0.080(11) Uani 1 1 d . A .
C1 C -0.002(3) 0.4338(10) 1.3112(16) 0.036(7) Uani 1 1 d . . .
N2 N 0.124(3) 0.3510(10) 1.479(2) 0.062(8) Uani 1 1 d . A .
C2 C 0.023(3) 0.3705(11) 1.4398(19) 0.043(8) Uani 1 1 d . . .
N3 N -0.363(3) 0.3466(12) 1.478(2) 0.069(9) Uani 1 1 d . A .
C3 C -0.278(3) 0.3652(10) 1.4391(17) 0.035(7) Uani 1 1 d . . .
N4 N -0.407(3) 0.4475(11) 1.2720(17) 0.053(8) Uani 1 1 d . . .
C4 C -0.307(3) 0.4287(10) 1.3083(18) 0.032(6) Uani 1 1 d . . .
N5 N 0.489(3) 0.5301(10) 1.1774(16) 0.052(8) Uani 1 1 d . A .
C5 C 0.525(4) 0.5612(13) 1.1443(18) 0.047(8) Uani 1 1 d . . .
N6 N 0.604(4) 0.6687(11) 1.2584(19) 0.073(9) Uani 1 1 d . A .
C6 C 0.601(4) 0.6526(11) 1.1911(19) 0.048(8) Uani 1 1 d . . .
N7 N 0.664(4) 0.7103(10) 0.9819(17) 0.063(9) Uani 1 1 d . A .
C7 C 0.637(5) 0.6764(14) 1.016(2) 0.068(12) Uani 1 1 d . . .
N8 N 0.572(5) 0.5673(8) 0.904(2) 0.097(15) Uani 1 1 d . . .
C8 C 0.567(4) 0.5874(9) 0.9660(18) 0.045(9) Uani 1 1 d . . .
N4H N 0.618(3) 0.6952(7) 1.4381(15) 0.038(6) Uani 1 1 d . . .
O10 O 0.357(3) 0.4726(11) 1.3793(14) 0.083(9) Uani 1 1 d DU A .
C11 C 0.411(4) 0.4534(8) 1.4476(15) 0.059(11) Uani 1 1 d DU . .
N12 N 0.349(3) 0.4550(10) 1.5201(15) 0.066(9) Uani 1 1 d DU A .
C13 C 0.211(4) 0.4836(18) 1.515(2) 0.098(17) Uani 1 1 d DU . .
C14 C 0.410(5) 0.4289(17) 1.5965(18) 0.13(2) Uani 1 1 d DU . .
O20 O 0.245(3) 0.5377(10) 1.271(2) 0.101(12) Uani 1 1 d DU A .
C21 C 0.247(6) 0.5802(14) 1.254(3) 0.19(3) Uani 1 1 d DU . .
N22 N 0.142(4) 0.6031(13) 1.2962(17) 0.123(17) Uani 1 1 d DU A .
C23 C 0.114(11) 0.5678(17) 1.370(5) 0.49(9) Uani 1 1 d DU . .
C24 C 0.197(8) 0.6499(13) 1.321(4) 0.20(4) Uani 1 1 d DU . .
O30 O 0.184(3) 0.4882(18) 1.102(3) 0.18(2) Uani 1 1 d DU A .
C31 C 0.218(7) 0.5273(16) 1.071(5) 0.14(3) Uani 0.36(7) 1 d PDU A 1
N32 N 0.125(6) 0.5422(15) 1.006(3) 0.049(18) Uani 0.36(7) 1 d PDU A 1
C33 C 0.008(9) 0.571(3) 1.050(4) 0.06(3) Uani 0.36(7) 1 d PDU A 1
C34 C 0.191(10) 0.555(3) 0.926(4) 0.18(5) Uani 0.36(7) 1 d PDU A 1
C35 C 0.250(6) 0.509(2) 1.040(3) 0.14(3) Uani 0.64(7) 1 d PDU A 2
N36 N 0.154(7) 0.521(3) 0.973(3) 0.20(4) Uani 0.64(7) 1 d PDU A 2
C37 C 0.036(10) 0.549(4) 1.019(4) 0.24(6) Uani 0.64(7) 1 d PDU A 2
C38 C 0.219(9) 0.536(3) 0.894(3) 0.16(4) Uani 0.64(7) 1 d PDU A 2
O40 O 0.331(3) 0.3909(10) 1.2499(16) 0.090(10) Uani 1 1 d DU A .
C41 C 0.450(5) 0.3669(16) 1.262(18) 2.0(9) Uani 1 1 d DU A .
N42 N 0.422(6) 0.3222(14) 1.266(3) 0.22(3) Uani 1 1 d DU . .
C43 C 0.548(7) 0.297(4) 1.228(5) 0.52(11) Uani 1 1 d DU A .
C44 C 0.270(8) 0.309(2) 1.272(5) 0.23(5) Uani 1 1 d DU A .
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'
Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pt Pt -1.7033 8.3905 '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
O20 Yb O10 71.1(11) . . ?
O20 Yb O40 143.6(10) . . ?
O10 Yb O40 83.5(10) . . ?
O20 Yb O30 80.8(16) . . ?
O10 Yb O30 144.4(14) . . ?
O40 Yb O30 109.0(14) . . ?
O20 Yb N5 72.0(10) . . ?
O10 Yb N5 107.2(10) . . ?
O40 Yb N5 142.4(11) . . ?
O30 Yb N5 83.4(10) . . ?
O20 Yb N1 74.5(11) . . ?
O10 Yb N1 75.5(9) . . ?
O40 Yb N1 74.1(12) . . ?
O30 Yb N1 76.3(10) . . ?
N5 Yb N1 143.1(11) . . ?
O20 Yb N4 120.7(10) . 1_655 ?
O10 Yb N4 74.5(9) . 1_655 ?
O40 Yb N4 74.3(10) . 1_655 ?
O30 Yb N4 140.4(12) . 1_655 ?
N5 Yb N4 74.3(10) . 1_655 ?
N1 Yb N4 138.3(10) . 1_655 ?
O20 Yb N8 140.6(10) . 3_667 ?
O10 Yb N8 145.4(9) . 3_667 ?
O40 Yb N8 72.6(9) . 3_667 ?
O30 Yb N8 68.9(15) . 3_667 ?
N5 Yb N8 79.8(10) . 3_667 ?
N1 Yb N8 119.4(11) . 3_667 ?
N4 Yb N8 75.2(10) 1_655 3_667 ?
O20 Yb C31 68.9(15) . . ?
O10 Yb C31 140.0(15) . . ?
O40 Yb C31 130.2(12) . . ?
O30 Yb C31 22.9(11) . . ?
N5 Yb C31 61.5(12) . . ?
N1 Yb C31 92.2(15) . . ?
N4 Yb C31 129.2(15) 1_655 . ?
N8 Yb C31 73.7(15) 3_667 . ?
O20 Yb C35 83.4(16) . . ?
O10 Yb C35 154.4(16) . . ?
O40 Yb C35 119.0(14) . . ?
O30 Yb C35 22.0(10) . . ?
N5 Yb C35 63.2(10) . . ?
N1 Yb C35 98.0(12) . . ?
N4 Yb C35 121.0(13) 1_655 . ?
N8 Yb C35 59.3(15) 3_667 . ?
C31 Yb C35 14.5(18) . . ?
O20 Yb C41 153(5) . . ?
O10 Yb C41 82(5) . . ?
O40 Yb C41 20.0(10) . . ?
O30 Yb C41 120(4) . . ?
N5 Yb C41 124(2) . . ?
N1 Yb C41 93(2) . . ?
N4 Yb C41 54.7(13) 1_655 . ?
N8 Yb C41 67(5) 3_667 . ?
C31 Yb C41 137(5) . . ?
C35 Yb C41 123(5) . . ?
C2 Pt1 C1 89.9(13) . . ?
C2 Pt1 C3 90.5(12) . . ?
C1 Pt1 C3 178.2(12) . . ?
C2 Pt1 C4 178.5(13) . . ?
C1 Pt1 C4 90.8(12) . . ?
C3 Pt1 C4 88.8(12) . . ?
C8 Pt2 C6 177.1(14) . . ?
C8 Pt2 C7 88.3(11) . . ?
C6 Pt2 C7 90.0(13) . . ?
C8 Pt2 C5 92.6(10) . . ?
C6 Pt2 C5 89.0(12) . . ?
C7 Pt2 C5 176.4(16) . . ?
C1 N1 Yb 155(3) . . ?
N1 C1 Pt1 175(3) . . ?
N2 C2 Pt1 177(3) . . ?
N3 C3 Pt1 178(3) . . ?
C4 N4 Yb 160(2) . 1_455 ?
N4 C4 Pt1 178(3) . . ?
C5 N5 Yb 162(3) . . ?
N5 C5 Pt2 178(3) . . ?
N6 C6 Pt2 174(3) . . ?
N7 C7 Pt2 178(3) . . ?
C8 N8 Yb 163(4) . 3_667 ?
N8 C8 Pt2 171(3) . . ?
C11 O10 Yb 145(2) . . ?
O10 C11 N12 123(3) . . ?
C11 N12 C14 120.5(12) . . ?
C11 N12 C13 113(2) . . ?
C14 N12 C13 126(2) . . ?
C21 O20 Yb 141(3) . . ?
O20 C21 N22 111(3) . . ?
C21 N22 C24 110(3) . . ?
C21 N22 C23 100(3) . . ?
C24 N22 C23 119(3) . . ?
C31 O30 C35 35(4) . . ?
C31 O30 Yb 111(3) . . ?
C35 O30 Yb 116(2) . . ?
O30 C31 N32 115(4) . . ?
O30 C31 Yb 46(2) . . ?
N32 C31 Yb 159(3) . . ?
C31 N32 C34 116(3) . . ?
C31 N32 C33 106(3) . . ?
C34 N32 C33 124(3) . . ?
O30 C35 N36 112(3) . . ?
O30 C35 Yb 42.3(17) . . ?
N36 C35 Yb 154(3) . . ?
C35 N36 C38 116(3) . . ?
C35 N36 C37 103(3) . . ?
C38 N36 C37 123(4) . . ?
C41 O40 Yb 122(3) . . ?
O40 C41 N42 112(3) . . ?
O40 C41 Yb 38(2) . . ?
N42 C41 Yb 150(4) . . ?
C41 N42 C44 117(2) . . ?
C41 N42 C43 108(3) . . ?
C44 N42 C43 130(4) . . ?
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
Yb O20 2.26(3) . ?
Yb O10 2.32(2) . ?
Yb O40 2.32(3) . ?
Yb O30 2.34(3) . ?
Yb N5 2.39(2) . ?
Yb N1 2.40(3) . ?
Yb N4 2.45(3) 1_655 ?
Yb N8 2.48(4) 3_667 ?
Yb C31 3.05(5) . ?
Yb C35 3.14(3) . ?
Yb C41 3.19(5) . ?
Pt1 C2 1.90(3) . ?
Pt1 C1 1.91(3) . ?
Pt1 C3 1.93(3) . ?
Pt1 C4 1.95(3) . ?
Pt2 C8 1.95(3) . ?
Pt2 C6 1.98(3) . ?
Pt2 C7 2.01(4) . ?
Pt2 C5 2.05(4) . ?
N1 C1 1.25(4) . ?
N2 C2 1.20(4) . ?
N3 C3 1.14(4) . ?
N4 C4 1.16(4) . ?
N4 Yb 2.45(3) 1_455 ?
N5 C5 1.10(4) . ?
N6 C6 1.13(4) . ?
N7 C7 1.15(4) . ?
N8 C8 1.13(4) . ?
N8 Yb 2.48(4) 3_667 ?
O10 C11 1.25(3) . ?
C11 N12 1.285(10) . ?
N12 C14 1.466(10) . ?
N12 C13 1.49(3) . ?
O20 C21 1.26(3) . ?
C21 N22 1.36(3) . ?
N22 C24 1.49(3) . ?
N22 C23 1.56(4) . ?
O30 C31 1.28(4) . ?
O30 C35 1.30(3) . ?
C31 N32 1.32(3) . ?
N32 C34 1.46(3) . ?
N32 C33 1.54(4) . ?
C35 N36 1.33(3) . ?
N36 C38 1.46(3) . ?
N36 C37 1.55(4) . ?
O40 C41 1.29(4) . ?
C41 N42 1.33(3) . ?
N42 C44 1.44(3) . ?
N42 C43 1.51(4) . ?
