#------------------------------------------------------------------------------
#$Date: 2016-03-24 14:27:18 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179664 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/17/4511798.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_4511798
loop_
_publ_author_name
'Bag, Prasenjit'
'Chakraborty, Amit'
'Rouzières, Mathieu'
'Clérac, Rodolphe'
'Butcher, Raymond J.'
'Chandrasekhar, Vadapalli'
_publ_section_title
;
 Oxalato-Bridged Neutral Octanuclear Heterometallic Complexes
 [Ln4K4(L)4(μ-H2O)4(NO3)2(μ-Ox)] (Ln = Dy(III), Gd(III), Tb(III),
 Ho(III); LH3= N[CH2CH2N═CH-C6H3-2-OH-3-OMe]3; Ox = (C2O4)2--):
 Synthesis, Structure, Magnetic and Luminescent Properties
;
_journal_issue                   9
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              4583
_journal_paper_doi               10.1021/cg500677t
_journal_volume                  14
_journal_year                    2014
_chemical_formula_moiety
'C122 H140 K4 N18 O38 Ho4, 4(C H4 O), 8(H2 O)'
_chemical_formula_sum            'C126 H172 Ho4 K4 N18 O50'
_chemical_formula_weight         3554.94
_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                90.000(5)
_cell_angle_beta                 107.326(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            2
_cell_length_a                   15.874(5)
_cell_length_b                   29.111(5)
_cell_length_c                   16.677(5)
_cell_measurement_reflns_used    9612
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.32
_cell_measurement_theta_min      2.23
_cell_volume                     7357(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0532
_diffrn_reflns_av_sigmaI/netI    0.0641
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            38480
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    2.331
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.635271
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.606
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3596
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.127
_refine_diff_density_min         -3.711
_refine_diff_density_rms         0.248
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.158
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     926
_refine_ls_number_reflns         13653
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.161
_refine_ls_R_factor_all          0.1027
_refine_ls_R_factor_gt           0.0857
_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)+(0.0893P)²+143.5997P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2238
_refine_ls_wR_factor_ref         0.2376
_reflns_number_gt                11249
_reflns_number_total             13653
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg500677t_si_001.cif
_cod_data_source_block           Ho4K4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' according to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4511795--4511798.cif.
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4511798
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
Ho1 Ho 0.07927(4) 0.128950(19) 0.17370(3) 0.027 Uani 1 1 d .
Ho2 Ho 0.38059(4) 0.119220(18) 0.45606(3) 0.025 Uani 1 1 d .
K1 K 0.28251(18) 0.12741(9) 0.10071(17) 0.030 Uani 1 1 d .
K2 K 0.1953(2) 0.05556(11) 0.5045(2) 0.046 Uani 1 1 d .
O11 O 0.1274(5) 0.1042(3) 0.3179(5) 0.029 Uani 1 1 d D
O12 O 0.3324(5) 0.1268(3) 0.3046(5) 0.025 Uani 1 1 d D
O28 O 0.7824(17) 0.2167(8) 0.6667(15) 0.160 Uani 1 1 d .
H28 H 0.7527 0.2279 0.6222 0.239 Uiso 1 1 calc R
O30 O 0.8204(9) 0.1119(6) 0.4275(7) 0.162 Uani 1 1 d G
H30D H 0.7920 0.0970 0.4549 0.243 Uiso 1 1 d G
H30E H 0.8629 0.0956 0.4223 0.243 Uiso 1 1 d G
O31 O 0.6447(13) 0.2080(6) 0.0413(7) 0.159 Uani 1 1 d G
H31E H 0.5908 0.2012 0.0334 0.239 Uiso 1 1 d G
H31F H 0.6754 0.1979 0.0888 0.239 Uiso 1 1 d G
O32 O 0.6992(8) 0.1351(4) 0.2565(7) 0.114 Uani 1 1 d G
H32E H 0.6818 0.1104 0.2293 0.170 Uiso 1 1 d G
H32F H 0.6550 0.1498 0.2617 0.170 Uiso 1 1 d G
O33 O 0.6963(13) 0.1717(8) 0.9223(7) 0.151 Uani 1 1 d G
H33C H 0.7019 0.1429 0.9299 0.226 Uiso 1 1 d G
H33D H 0.6583 0.1771 0.8752 0.226 Uiso 1 1 d G
O11A O 0.1051(6) 0.1230(3) 0.0482(5) 0.033 Uani 1 1 d .
O12A O 0.1916(6) 0.0874(3) -0.0473(5) 0.041 Uani 1 1 d .
O21A O 0.1901(5) 0.0756(3) 0.1900(5) 0.026 Uani 1 1 d .
O22A O 0.3510(6) 0.0492(3) 0.1936(5) 0.031 Uani 1 1 d .
O31A O 0.1977(5) 0.1772(3) 0.2024(5) 0.026 Uani 1 1 d .
O32A O 0.3371(6) 0.2113(3) 0.1656(6) 0.036 Uani 1 1 d .
O11B O 0.3717(6) 0.0793(3) 0.5701(5) 0.038 Uani 1 1 d .
O12B O 0.3073(9) 0.0141(4) 0.6450(8) 0.071 Uani 1 1 d .
O21B O 0.2448(5) 0.1422(3) 0.4571(5) 0.028 Uani 1 1 d .
O22B O 0.1164(6) 0.1326(3) 0.5276(7) 0.045 Uani 1 1 d .
O31B O 0.2957(5) 0.0566(3) 0.4003(5) 0.029 Uani 1 1 d .
O32B O 0.1499(6) 0.0067(3) 0.3523(6) 0.039 Uani 1 1 d .
O1N O 0.4410(8) 0.1148(4) 0.0612(8) 0.070 Uani 1 1 d .
O2N O 0.4981(12) 0.1573(7) -0.0111(12) 0.122 Uani 1 1 d .
O3N O 0.3597(9) 0.1604(4) -0.0228(9) 0.075 Uani 1 1 d .
O1OX O -0.0741(7) -0.0074(4) 0.4595(7) 0.052 Uani 1 1 d DU
O2OX O -0.0063(7) 0.0502(4) 0.4387(7) 0.053 Uani 1 1 d U
N1A N -0.0737(8) 0.1254(4) 0.2099(7) 0.044 Uani 1 1 d .
N12A N -0.0484(7) 0.1638(4) 0.0623(6) 0.037 Uani 1 1 d .
N22A N 0.0058(7) 0.0534(4) 0.1384(7) 0.036 Uani 1 1 d .
N32A N 0.0485(7) 0.1972(4) 0.2594(6) 0.036 Uani 1 1 d .
N1B N 0.5232(6) 0.1557(3) 0.4293(6) 0.028 Uani 1 1 d .
N11B N 0.3664(7) 0.2049(3) 0.4196(6) 0.028 Uani 1 1 d .
N22B N 0.4817(7) 0.1559(4) 0.5860(6) 0.032 Uani 1 1 d .
N32B N 0.4835(6) 0.0600(3) 0.4311(6) 0.028 Uani 1 1 d .
N1N N 0.4341(10) 0.1437(6) 0.0090(10) 0.069 Uani 1 1 d .
C18 C 0.3043(8) 0.0140(4) 0.3770(7) 0.026 Uani 1 1 d .
C10A C 0.2440(11) 0.0708(5) -0.0986(10) 0.051 Uani 1 1 d .
H10A H 0.2093 0.0504 -0.1408 0.076 Uiso 1 1 calc R
H10B H 0.2946 0.0547 -0.0640 0.076 Uiso 1 1 calc R
H10C H 0.2632 0.0963 -0.1251 0.076 Uiso 1 1 calc R
C20 C 0.4385(9) 0.0344(5) 0.1957(8) 0.037 Uani 1 1 d .
H20A H 0.4554 0.0085 0.2326 0.056 Uiso 1 1 calc R
H20B H 0.4796 0.0590 0.2157 0.056 Uiso 1 1 calc R
H20C H 0.4387 0.0258 0.1402 0.056 Uiso 1 1 calc R
C30 C 0.4122(9) 0.2292(5) 0.1476(8) 0.040 Uani 1 1 d .
H30A H 0.3939 0.2495 0.1002 0.059 Uiso 1 1 calc R
H30B H 0.4460 0.2044 0.1349 0.059 Uiso 1 1 calc R
H30C H 0.4478 0.2458 0.1954 0.059 Uiso 1 1 calc R
C40 C 0.275(2) -0.0219(9) 0.6868(15) 0.123 Uani 1 1 d .
H40A H 0.3229 -0.0331 0.7330 0.184 Uiso 1 1 calc R
H40B H 0.2529 -0.0465 0.6480 0.184 Uiso 1 1 calc R
H40C H 0.2293 -0.0102 0.7074 0.184 Uiso 1 1 calc R
C50 C 0.0466(13) 0.1271(6) 0.5636(14) 0.073 Uani 1 1 d .
H50A H 0.0481 0.1518 0.6022 0.110 Uiso 1 1 calc R
H50B H 0.0532 0.0984 0.5929 0.110 Uiso 1 1 calc R
H50C H -0.0088 0.1276 0.5200 0.110 Uiso 1 1 calc R
C60 C 0.0690(9) -0.0203(5) 0.3267(11) 0.050 Uani 1 1 d .
H60A H 0.0585 -0.0303 0.2697 0.075 Uiso 1 1 calc R
H60B H 0.0204 -0.0017 0.3307 0.075 Uiso 1 1 calc R
H60C H 0.0748 -0.0465 0.3628 0.075 Uiso 1 1 calc R
C11A C -0.1467(9) 0.1497(7) 0.1473(9) 0.053 Uani 1 1 d .
H11C H -0.1836 0.1650 0.1761 0.064 Uiso 1 1 calc R
H11D H -0.1828 0.1274 0.1089 0.064 Uiso 1 1 calc R
C12A C -0.1114(9) 0.1851(6) 0.0975(8) 0.050 Uani 1 1 d .
H12C H -0.1599 0.1976 0.0528 0.060 Uiso 1 1 calc R
H12D H -0.0834 0.2101 0.1342 0.060 Uiso 1 1 calc R
C13A C -0.0696(9) 0.1629(5) -0.0194(8) 0.037 Uani 1 1 d .
H13A H -0.1231 0.1762 -0.0490 0.044 Uiso 1 1 calc R
C14A C -0.0175(9) 0.1433(5) -0.0674(8) 0.035 Uani 1 1 d .
C15A C -0.0549(10) 0.1436(5) -0.1558(8) 0.042 Uani 1 1 d .
H15A H -0.1109 0.1560 -0.1788 0.050 Uiso 1 1 calc R
C16A C -0.0117(10) 0.1265(5) -0.2074(9) 0.046 Uani 1 1 d .
H16A H -0.0371 0.1283 -0.2652 0.056 Uiso 1 1 calc R
C17A C 0.0714(9) 0.1059(4) -0.1746(8) 0.038 Uani 1 1 d .
H17A H 0.0997 0.0928 -0.2104 0.046 Uiso 1 1 calc R
C18A C 0.1109(9) 0.1052(4) -0.0882(8) 0.034 Uani 1 1 d .
C19A C 0.0653(9) 0.1241(4) -0.0320(7) 0.030 Uani 1 1 d .
C21A C -0.1005(9) 0.0765(5) 0.2136(8) 0.041 Uani 1 1 d .
H21A H -0.1616 0.0748 0.2134 0.049 Uiso 1 1 calc R
H21B H -0.0640 0.0621 0.2646 0.049 Uiso 1 1 calc R
C22A C -0.0887(10) 0.0515(7) 0.1352(10) 0.058 Uani 1 1 d .
H22A H -0.1075 0.0198 0.1346 0.069 Uiso 1 1 calc R
H22B H -0.1246 0.0663 0.0844 0.069 Uiso 1 1 calc R
C23A C 0.0357(9) 0.0160(5) 0.1178(8) 0.039 Uani 1 1 d .
H23A H -0.0050 -0.0075 0.0991 0.047 Uiso 1 1 calc R
C24A C 0.1246(9) 0.0061(4) 0.1201(7) 0.034 Uani 1 1 d .
C25A C 0.1390(11) -0.0377(5) 0.0884(9) 0.048 Uani 1 1 d .
H25A H 0.0909 -0.0566 0.0644 0.058 Uiso 1 1 calc R
C26A C 0.2209(11) -0.0522(5) 0.0925(9) 0.052 Uani 1 1 d .
H26A H 0.2287 -0.0810 0.0717 0.063 Uiso 1 1 calc R
C27A C 0.2956(10) -0.0237(5) 0.1287(8) 0.043 Uani 1 1 d .
H27A H 0.3522 -0.0339 0.1323 0.051 Uiso 1 1 calc R
C28A C 0.2826(8) 0.0190(4) 0.1580(7) 0.027 Uani 1 1 d .
C29A C 0.1974(9) 0.0353(4) 0.1573(7) 0.031 Uani 1 1 d .
C31A C -0.0562(9) 0.1457(7) 0.2936(8) 0.053 Uani 1 1 d .
H31A H -0.0122 0.1273 0.3334 0.063 Uiso 1 1 calc R
H31B H -0.1099 0.1447 0.3100 0.063 Uiso 1 1 calc R
C32A C -0.0244(9) 0.1946(6) 0.2982(9) 0.046 Uani 1 1 d .
H32A H -0.0724 0.2146 0.2685 0.055 Uiso 1 1 calc R
H32B H -0.0036 0.2045 0.3563 0.055 Uiso 1 1 calc R
C33A C 0.0849(9) 0.2365(5) 0.2676(8) 0.040 Uani 1 1 d .
H33A H 0.0611 0.2584 0.2953 0.049 Uiso 1 1 calc R
C34A C 0.1579(9) 0.2518(4) 0.2398(8) 0.039 Uani 1 1 d .
C35A C 0.1781(11) 0.3006(5) 0.2481(9) 0.052 Uani 1 1 d .
H35A H 0.1433 0.3203 0.2687 0.063 Uiso 1 1 calc R
C36A C 0.2481(11) 0.3176(5) 0.2257(9) 0.050 Uani 1 1 d .
H36A H 0.2604 0.3489 0.2311 0.061 Uiso 1 1 calc R
C37A C 0.3006(10) 0.2891(4) 0.1955(8) 0.040 Uani 1 1 d .
H37A H 0.3468 0.3012 0.1786 0.048 Uiso 1 1 calc R
C38A C 0.2845(8) 0.2422(4) 0.1903(7) 0.032 Uani 1 1 d .
C39A C 0.2115(8) 0.2226(4) 0.2101(7) 0.031 Uani 1 1 d .
C11B C 0.5838(8) 0.1752(5) 0.5074(8) 0.034 Uani 1 1 d .
H11E H 0.6156 0.2008 0.4927 0.041 Uiso 1 1 calc R
H11F H 0.6267 0.1520 0.5343 0.041 Uiso 1 1 calc R
C12B C 0.5370(9) 0.1919(5) 0.5695(8) 0.040 Uani 1 1 d .
H12E H 0.5804 0.2009 0.6216 0.048 Uiso 1 1 calc R
H12F H 0.5012 0.2186 0.5468 0.048 Uiso 1 1 calc R
C13B C 0.4904(10) 0.1481(5) 0.6653(8) 0.043 Uani 1 1 d .
H13B H 0.5297 0.1671 0.7035 0.052 Uiso 1 1 calc R
C14B C 0.4467(10) 0.1135(5) 0.7012(8) 0.040 Uani 1 1 d .
C15B C 0.4690(12) 0.1128(6) 0.7907(9) 0.056 Uani 1 1 d .
H15B H 0.5046 0.1355 0.8228 0.067 Uiso 1 1 calc R
C16B C 0.4370(12) 0.0779(7) 0.8284(10) 0.064 Uani 1 1 d .
H16B H 0.4522 0.0768 0.8867 0.076 Uiso 1 1 calc R
C17B C 0.3839(12) 0.0451(6) 0.7828(10) 0.059 Uani 1 1 d .
H17B H 0.3631 0.0218 0.8100 0.071 Uiso 1 1 calc R
C18B C 0.3602(11) 0.0458(5) 0.6967(10) 0.050 Uani 1 1 d .
C19B C 0.3908(9) 0.0809(5) 0.6512(8) 0.039 Uani 1 1 d .
C21B C 0.4904(9) 0.1918(4) 0.3634(8) 0.035 Uani 1 1 d .
H21C H 0.5406 0.2069 0.3530 0.042 Uiso 1 1 calc R
H21D H 0.4566 0.1771 0.3116 0.042 Uiso 1 1 calc R
C22B C 0.4344(9) 0.2270(4) 0.3867(7) 0.033 Uani 1 1 d .
H22C H 0.4055 0.2455 0.3378 0.040 Uiso 1 1 calc R
H22D H 0.4711 0.2472 0.4292 0.040 Uiso 1 1 calc R
C23B C 0.3067(8) 0.2332(4) 0.4237(7) 0.031 Uani 1 1 d .
H23B H 0.3104 0.2626 0.4031 0.037 Uiso 1 1 calc R
C24B C 0.2321(9) 0.2244(4) 0.4575(7) 0.034 Uani 1 1 d .
C25B C 0.1849(9) 0.2630(4) 0.4722(8) 0.037 Uani 1 1 d .
H25B H 0.1995 0.2921 0.4575 0.044 Uiso 1 1 calc R
C26B C 0.1197(9) 0.2584(5) 0.5071(8) 0.043 Uani 1 1 d .
H26B H 0.0916 0.2844 0.5190 0.052 Uiso 1 1 calc R
C27B C 0.0935(9) 0.2157(5) 0.5255(8) 0.038 Uani 1 1 d .
H27B H 0.0468 0.2128 0.5481 0.046 Uiso 1 1 calc R
C28B C 0.1380(8) 0.1765(5) 0.5099(8) 0.035 Uani 1 1 d .
C29B C 0.2065(9) 0.1803(4) 0.4742(8) 0.033 Uani 1 1 d .
C31B C 0.5716(8) 0.1197(4) 0.3954(8) 0.035 Uani 1 1 d .
H31C H 0.6311 0.1301 0.4007 0.042 Uiso 1 1 calc R
H31D H 0.5416 0.1143 0.3364 0.042 Uiso 1 1 calc R
C32B C 0.5747(8) 0.0759(4) 0.4444(8) 0.032 Uani 1 1 d .
H32C H 0.6082 0.0527 0.4253 0.039 Uiso 1 1 calc R
H32D H 0.6031 0.0814 0.5037 0.039 Uiso 1 1 calc R
C33B C 0.4676(8) 0.0184(4) 0.4026(7) 0.028 Uani 1 1 d .
H33B H 0.5163 0.0018 0.3986 0.034 Uiso 1 1 calc R
C34B C 0.3842(8) -0.0056(4) 0.3764(7) 0.029 Uani 1 1 d .
C35B C 0.3873(9) -0.0509(4) 0.3459(8) 0.038 Uani 1 1 d .
H35B H 0.4409 -0.0632 0.3445 0.046 Uiso 1 1 calc R
C36B C 0.3119(8) -0.0768(4) 0.3184(7) 0.033 Uani 1 1 d .
H36B H 0.3149 -0.1068 0.2999 0.039 Uiso 1 1 calc R
C37B C 0.2317(9) -0.0584(4) 0.3184(8) 0.036 Uani 1 1 d .
H37B H 0.1803 -0.0755 0.2982 0.043 Uiso 1 1 calc R
C38B C 0.2280(8) -0.0139(4) 0.3486(8) 0.029 Uani 1 1 d .
C1OX C -0.0167(14) 0.0134(7) 0.4758(15) 0.092 Uani 1 1 d D
H11A H 0.172(8) 0.087(6) 0.319(12) 0.110 Uiso 1 1 d D
H11B H 0.151(12) 0.119(6) 0.363(8) 0.110 Uiso 1 1 d D
H12A H 0.316(11) 0.104(4) 0.274(11) 0.110 Uiso 1 1 d D
H12B H 0.274(5) 0.138(7) 0.291(13) 0.110 Uiso 1 1 d D
O34 O 0.6120(10) 0.0756(6) 0.1241(9) 0.093 Uani 1 1 d .
H34 H 0.6562 0.0827 0.1622 0.140 Uiso 1 1 calc R
C83 C 0.6370(10) 0.0602(5) 0.0553(10) 0.050 Uani 1 1 d .
H83A H 0.6482 0.0861 0.0243 0.075 Uiso 1 1 calc R
H83B H 0.5904 0.0419 0.0196 0.075 Uiso 1 1 calc R
H83C H 0.6896 0.0420 0.0746 0.075 Uiso 1 1 calc R
C84 C 0.7900(10) 0.1700(5) 0.6569(10) 0.050 Uani 1 1 d .
H84A H 0.8269 0.1643 0.6216 0.075 Uiso 1 1 calc R
H84B H 0.7326 0.1571 0.6314 0.075 Uiso 1 1 calc R
H84C H 0.8158 0.1561 0.7108 0.075 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'
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'
Ho Ho -0.2175 4.6783 '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
O11A Ho1 O31A 82.8(3) . .
O11A Ho1 O21A 73.4(3) . .
O31A Ho1 O21A 80.7(3) . .
O11A Ho1 O11 144.4(3) . .
O31A Ho1 O11 88.8(3) . .
O21A Ho1 O11 71.1(3) . .
O11A Ho1 N22A 85.1(3) . .
O31A Ho1 N22A 153.8(3) . .
O21A Ho1 N22A 73.6(3) . .
O11 Ho1 N22A 87.6(3) . .
O11A Ho1 N12A 71.0(3) . .
O31A Ho1 N12A 109.7(3) . .
O21A Ho1 N12A 141.1(3) . .
O11 Ho1 N12A 143.5(3) . .
N22A Ho1 N12A 88.0(4) . .
O11A Ho1 N32A 133.6(3) . .
O31A Ho1 N32A 71.9(3) . .
O21A Ho1 N32A 136.0(3) . .
O11 Ho1 N32A 74.5(3) . .
N22A Ho1 N32A 131.5(4) . .
N12A Ho1 N32A 81.6(3) . .
O11A Ho1 N1A 129.4(3) . .
O31A Ho1 N1A 136.4(3) . .
O21A Ho1 N1A 131.4(3) . .
O11 Ho1 N1A 78.6(3) . .
N22A Ho1 N1A 67.9(4) . .
N12A Ho1 N1A 66.2(4) . .
N32A Ho1 N1A 64.5(4) . .
O11A Ho1 K1 44.8(2) . .
O31A Ho1 K1 49.0(2) . .
O21A Ho1 K1 48.18(19) . .
O11 Ho1 K1 105.7(2) . .
N22A Ho1 K1 107.5(2) . .
N12A Ho1 K1 110.1(2) . .
N32A Ho1 K1 120.6(3) . .
N1A Ho1 K1 173.8(3) . .
O21B Ho2 O11B 81.3(3) . .
O21B Ho2 O31B 78.0(3) . .
O11B Ho2 O31B 75.9(3) . .
O21B Ho2 O12 88.6(3) . .
O11B Ho2 O12 147.3(3) . .
O31B Ho2 O12 71.6(3) . .
O21B Ho2 N32B 151.5(3) . .
O11B Ho2 N32B 89.6(3) . .
O31B Ho2 N32B 73.6(3) . .
O12 Ho2 N32B 84.7(3) . .
O21B Ho2 N22B 103.4(3) . .
O11B Ho2 N22B 71.3(3) . .
O31B Ho2 N22B 146.4(3) . .
O12 Ho2 N22B 141.4(3) . .
N32B Ho2 N22B 99.0(3) . .
O21B Ho2 N11B 72.3(3) . .
O11B Ho2 N11B 132.5(3) . .
O31B Ho2 N11B 132.7(3) . .
O12 Ho2 N11B 71.7(3) . .
N32B Ho2 N11B 130.5(3) . .
N22B Ho2 N11B 77.3(3) . .
O21B Ho2 N1B 138.1(3) . .
O11B Ho2 N1B 127.9(3) . .
O31B Ho2 N1B 132.6(3) . .
O12 Ho2 N1B 79.0(3) . .
N32B Ho2 N1B 67.4(3) . .
N22B Ho2 N1B 67.6(3) . .
N11B Ho2 N1B 65.8(3) . .
O21B Ho2 K2 48.4(2) . .
O11B Ho2 K2 47.2(2) . .
O31B Ho2 K2 45.0(2) . .
O12 Ho2 K2 104.15(19) . .
N32B Ho2 K2 106.7(2) . .
N22B Ho2 K2 111.3(2) . .
N11B Ho2 K2 120.8(2) . .
N1B Ho2 K2 173.3(2) . .
O11A K1 O32A 110.6(3) . .
O11A K1 O12A 57.6(3) . .
O32A K1 O12A 140.3(3) . .
O11A K1 O22A 109.8(3) . .
O32A K1 O22A 119.3(3) . .
O12A K1 O22A 99.7(3) . .
O11A K1 O1N 147.3(4) . .
O32A K1 O1N 90.5(4) . .
O12A K1 O1N 90.1(4) . .
O22A K1 O1N 78.2(3) . .
O11A K1 O21A 59.2(2) . .
O32A K1 O21A 115.2(3) . .
O12A K1 O21A 91.8(3) . .
O22A K1 O21A 56.4(2) . .
O1N K1 O21A 134.2(3) . .
O11A K1 O31A 65.4(2) . .
O32A K1 O31A 57.0(2) . .
O12A K1 O31A 122.6(3) . .
O22A K1 O31A 105.1(2) . .
O1N K1 O31A 145.0(4) . .
O21A K1 O31A 63.0(2) . .
O11A K1 O3N 114.4(4) . .
O32A K1 O3N 80.2(3) . .
O12A K1 O3N 73.5(4) . .
O22A K1 O3N 119.7(3) . .
O1N K1 O3N 43.0(4) . .
O21A K1 O3N 164.3(3) . .
O31A K1 O3N 129.5(3) . .
O11A K1 N1N 134.7(4) . .
O32A K1 N1N 82.1(4) . .
O12A K1 N1N 84.4(4) . .
O22A K1 N1N 99.2(4) . .
O1N K1 N1N 21.1(4) . .
O21A K1 N1N 154.4(4) . .
O31A K1 N1N 138.8(3) . .
O3N K1 N1N 22.3(4) . .
O11A K1 O12 104.2(2) . .
O32A K1 O12 68.8(2) . .
O12A K1 O12 147.5(3) . .
O22A K1 O12 58.7(2) . .
O1N K1 O12 106.7(3) . .
O21A K1 O12 56.5(2) . .
O31A K1 O12 52.7(2) . .
O3N K1 O12 137.0(3) . .
N1N K1 O12 120.6(3) . .
O11A K1 Ho1 36.19(17) . .
O32A K1 Ho1 93.6(2) . .
O12A K1 Ho1 91.4(2) . .
O22A K1 Ho1 93.45(18) . .
O1N K1 Ho1 171.6(2) . .
O21A K1 Ho1 37.48(16) . .
O31A K1 Ho1 37.11(16) . .
O3N K1 Ho1 145.1(3) . .
N1N K1 Ho1 167.2(3) . .
O12 K1 Ho1 68.18(15) . .
O1OX K2 O22B 90.5(3) 3_556 .
O1OX K2 O31B 141.3(3) 3_556 .
O22B K2 O31B 118.8(3) . .
O1OX K2 O12B 84.4(4) 3_556 .
O22B K2 O12B 117.3(4) . .
O31B K2 O12B 101.4(3) . .
O1OX K2 O11B 140.8(3) 3_556 .
O22B K2 O11B 101.4(3) . .
O31B K2 O11B 61.9(3) . .
O12B K2 O11B 57.0(3) . .
O1OX K2 O32B 85.8(3) 3_556 .
O22B K2 O32B 123.7(3) . .
O31B K2 O32B 57.5(3) . .
O12B K2 O32B 118.2(4) . .
O11B K2 O32B 116.1(3) . .
O1OX K2 O21B 146.7(3) 3_556 .
O22B K2 O21B 57.9(3) . .
O31B K2 O21B 62.6(2) . .
O12B K2 O21B 117.7(3) . .
O11B K2 O21B 63.6(3) . .
O32B K2 O21B 102.5(3) . .
O1OX K2 O2OX 44.5(3) 3_556 .
O22B K2 O2OX 66.9(3) . .
O31B K2 O2OX 121.8(3) . .
O12B K2 O2OX 128.4(3) . .
O11B K2 O2OX 168.2(3) . .
O32B K2 O2OX 72.0(3) . .
O21B K2 O2OX 107.1(3) . .
O1OX K2 O11 113.2(3) 3_556 .
O22B K2 O11 74.8(3) . .
O31B K2 O11 58.3(2) . .
O12B K2 O11 159.4(3) . .
O11B K2 O11 105.9(2) . .
O32B K2 O11 56.0(2) . .
O21B K2 O11 52.5(2) . .
O2OX K2 O11 70.8(3) . .
O1OX K2 C1OX 24.0(4) 3_556 .
O22B K2 C1OX 80.7(4) . .
O31B K2 C1OX 130.6(5) . .
O12B K2 C1OX 108.3(4) . .
O11B K2 C1OX 164.6(4) . .
O32B K2 C1OX 73.7(5) . .
O21B K2 C1OX 127.9(4) . .
O2OX K2 C1OX 21.2(4) . .
O11 K2 C1OX 89.5(4) . .
O1OX K2 Ho2 176.5(3) 3_556 .
O22B K2 Ho2 92.7(2) . .
O31B K2 Ho2 37.15(18) . .
O12B K2 Ho2 92.9(3) . .
O11B K2 Ho2 36.87(17) . .
O32B K2 Ho2 93.54(18) . .
O21B K2 Ho2 36.80(17) . .
O2OX K2 Ho2 138.5(2) . .
O11 K2 Ho2 69.04(15) . .
C1OX K2 Ho2 158.5(4) . .
Ho1 O11 K2 171.8(3) . .
Ho2 O12 K1 173.6(3) . .
C19A O11A Ho1 141.9(8) . .
C19A O11A K1 118.3(7) . .
Ho1 O11A K1 99.0(3) . .
C18A O12A C10A 117.0(11) . .
C18A O12A K1 117.1(7) . .
C10A O12A K1 115.9(9) . .
C29A O21A Ho1 135.4(8) . .
C29A O21A K1 97.7(6) . .
Ho1 O21A K1 94.3(3) . .
C28A O22A C20 116.5(9) . .
C28A O22A K1 98.8(6) . .
C20 O22A K1 118.1(7) . .
C39A O31A Ho1 136.8(7) . .
C39A O31A K1 117.8(7) . .
Ho1 O31A K1 93.9(3) . .
C38A O32A C30 116.8(10) . .
C38A O32A K1 124.1(7) . .
C30 O32A K1 115.9(8) . .
C19B O11B Ho2 143.4(9) . .
C19B O11B K2 108.4(8) . .
Ho2 O11B K2 96.0(3) . .
C18B O12B C40 115.3(15) . .
C18B O12B K2 111.0(9) . .
C40 O12B K2 120.1(15) . .
C29B O21B Ho2 138.0(8) . .
C29B O21B K2 119.9(7) . .
Ho2 O21B K2 94.8(3) . .
C28B O22B C50 118.1(11) . .
C28B O22B K2 126.5(7) . .
C50 O22B K2 115.4(9) . .
C18 O31B Ho2 140.1(7) . .
C18 O31B K2 108.3(6) . .
Ho2 O31B K2 97.8(3) . .
C38B O32B C60 118.2(10) . .
C38B O32B K2 105.4(7) . .
C60 O32B K2 120.3(8) . .
N1N O1N K1 100.7(10) . .
N1N O3N K1 96.8(10) . .
C1OX O1OX C1OX 47.8(18) . 3_556
C1OX O1OX K2 153.0(16) . 3_556
C1OX O1OX K2 112.5(10) 3_556 3_556
C1OX O2OX K2 98.2(11) . .
C31A N1A C11A 111.4(12) . .
C31A N1A C21A 108.6(11) . .
C11A N1A C21A 108.0(12) . .
C31A N1A Ho1 105.9(8) . .
C11A N1A Ho1 113.2(8) . .
C21A N1A Ho1 109.6(8) . .
C13A N12A C12A 116.1(11) . .
C13A N12A Ho1 131.6(9) . .
C12A N12A Ho1 112.1(8) . .
C23A N22A C22A 114.4(12) . .
C23A N22A Ho1 129.4(9) . .
C22A N22A Ho1 116.1(10) . .
C33A N32A C32A 112.8(11) . .
C33A N32A Ho1 126.7(9) . .
C32A N32A Ho1 120.1(9) . .
C11B N1B C21B 111.6(10) . .
C11B N1B C31B 109.0(9) . .
C21B N1B C31B 108.6(9) . .
C11B N1B Ho2 111.6(7) . .
C21B N1B Ho2 106.0(7) . .
C31B N1B Ho2 109.9(7) . .
C23B N11B C22B 111.9(10) . .
C23B N11B Ho2 129.2(8) . .
C22B N11B Ho2 118.9(7) . .
C13B N22B C12B 115.5(11) . .
C13B N22B Ho2 130.1(10) . .
C12B N22B Ho2 114.3(7) . .
C33B N32B C32B 115.0(10) . .
C33B N32B Ho2 129.9(8) . .
C32B N32B Ho2 114.9(7) . .
O1N N1N O2N 121.6(17) . .
O1N N1N O3N 117.3(14) . .
O2N N1N O3N 121.1(18) . .
O1N N1N K1 58.2(8) . .
O2N N1N K1 165.0(15) . .
O3N N1N K1 60.9(8) . .
O31B C18 C34B 124.2(11) . .
O31B C18 C38B 118.9(10) . .
C34B C18 C38B 116.9(11) . .
N1A C11A C12A 111.5(11) . .
N12A C12A C11A 110.1(13) . .
N12A C13A C14A 125.5(13) . .
C19A C14A C15A 119.7(12) . .
C19A C14A C13A 123.8(11) . .
C15A C14A C13A 116.6(13) . .
C16A C15A C14A 121.9(14) . .
C15A C16A C17A 120.5(13) . .
C18A C17A C16A 119.5(12) . .
O12A C18A C17A 126.3(11) . .
O12A C18A C19A 113.3(11) . .
C17A C18A C19A 120.4(12) . .
O11A C19A C14A 123.7(11) . .
O11A C19A C18A 118.2(12) . .
C14A C19A C18A 118.0(11) . .
N1A C21A C22A 107.7(11) . .
N22A C22A C21A 109.1(11) . .
N22A C23A C24A 127.5(12) . .
C29A C24A C25A 119.9(13) . .
C29A C24A C23A 124.0(11) . .
C25A C24A C23A 115.8(12) . .
C26A C25A C24A 121.3(14) . .
C25A C26A C27A 120.5(13) . .
C28A C27A C26A 118.9(14) . .
C27A C28A O22A 123.0(12) . .
C27A C28A C29A 122.6(12) . .
O22A C28A C29A 114.3(10) . .
O21A C29A C24A 123.7(12) . .
O21A C29A C28A 119.5(11) . .
C24A C29A C28A 116.7(11) . .
N1A C31A C32A 113.3(12) . .
N32A C32A C31A 108.6(11) . .
N32A C33A C34A 128.9(12) . .
C39A C34A C33A 124.1(12) . .
C39A C34A C35A 119.3(14) . .
C33A C34A C35A 116.5(13) . .
C36A C35A C34A 120.2(14) . .
C35A C36A C37A 120.8(13) . .
C36A C37A C38A 119.9(14) . .
O32A C38A C37A 123.2(12) . .
O32A C38A C39A 114.8(10) . .
C37A C38A C39A 122.0(13) . .
O31A C39A C34A 122.4(11) . .
O31A C39A C38A 119.8(11) . .
C34A C39A C38A 117.8(11) . .
N1B C11B C12B 113.5(10) . .
N22B C12B C11B 110.2(11) . .
N22B C13B C14B 128.3(14) . .
C19B C14B C15B 122.0(14) . .
C19B C14B C13B 121.6(11) . .
C15B C14B C13B 116.3(14) . .
C16B C15B C14B 118.8(17) . .
C17B C16B C15B 121.4(15) . .
C16B C17B C18B 120.6(16) . .
O12B C18B C17B 125.1(15) . .
O12B C18B C19B 112.8(13) . .
C17B C18B C19B 122.1(17) . .
O11B C19B C14B 123.9(12) . .
O11B C19B C18B 120.9(14) . .
C14B C19B C18B 115.0(12) . .
C22B C21B N1B 113.5(10) . .
C21B C22B N11B 110.7(10) . .
N11B C23B C24B 127.1(11) . .
C29B C24B C25B 119.7(12) . .
C29B C24B C23B 123.2(11) . .
C25B C24B C23B 117.1(12) . .
C26B C25B C24B 121.1(13) . .
C25B C26B C27B 120.8(12) . .
C26B C27B C28B 119.4(12) . .
O22B C28B C29B 116.2(11) . .
O22B C28B C27B 122.8(12) . .
C29B C28B C27B 121.0(13) . .
O21B C29B C28B 119.3(12) . .
O21B C29B C24B 122.7(11) . .
C28B C29B C24B 117.9(11) . .
N1B C31B C32B 108.9(10) . .
N32B C32B C31B 108.2(10) . .
N32B C33B C34B 128.4(11) . .
C18 C34B C35B 120.8(12) . .
C18 C34B C33B 123.7(11) . .
C35B C34B C33B 115.5(11) . .
C36B C35B C34B 120.7(12) . .
C35B C36B C37B 119.8(12) . .
C36B C37B C38B 119.9(12) . .
O32B C38B C37B 123.3(11) . .
O32B C38B C18 114.9(10) . .
C37B C38B C18 121.8(11) . .
O1OX C1OX C1OX 88(2) . 3_556
O1OX C1OX O2OX 126(2) . .
C1OX C1OX O2OX 146(3) 3_556 .
O1OX C1OX O1OX 132.2(18) . 3_556
C1OX C1OX O1OX 43.7(13) 3_556 3_556
O2OX C1OX O1OX 102.0(15) . 3_556
O1OX C1OX K2 164(2) . .
C1OX C1OX K2 85(2) 3_556 .
O2OX C1OX K2 60.6(9) . .
O1OX C1OX K2 43.5(8) 3_556 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ho1 O11A 2.255(8) .
Ho1 O31A 2.281(8) .
Ho1 O21A 2.302(8) .
Ho1 O11 2.406(8) .
Ho1 N22A 2.478(11) .
Ho1 N12A 2.520(10) .
Ho1 N32A 2.579(11) .
Ho1 N1A 2.672(11) .
Ho1 K1 3.772(3) .
Ho2 O21B 2.261(8) .
Ho2 O11B 2.269(8) .
Ho2 O31B 2.293(8) .
Ho2 O12 2.422(8) .
Ho2 N32B 2.495(10) .
Ho2 N22B 2.518(10) .
Ho2 N11B 2.562(10) .
Ho2 N1B 2.656(10) .
Ho2 K2 3.762(3) .
K1 O11A 2.692(9) .
K1 O32A 2.708(9) .
K1 O12A 2.723(10) .
K1 O22A 2.787(9) .
K1 O1N 2.808(12) .
K1 O21A 2.819(8) .
K1 O31A 2.855(8) .
K1 O3N 2.858(13) .
K1 N1N 3.247(14) .
K1 O12 3.253(8) .
K2 O1OX 2.592(11) 3_556
K2 O22B 2.653(10) .
K2 O31B 2.686(8) .
K2 O12B 2.762(13) .
K2 O11B 2.773(10) .
K2 O32B 2.809(10) .
K2 O21B 2.824(9) .
K2 O2OX 3.063(11) .
K2 O11 3.295(9) .
K2 C1OX 3.48(2) .
O28 C84 1.38(3) .
O11A C19A 1.299(14) .
O12A C18A 1.361(16) .
O12A C10A 1.443(16) .
O21A C29A 1.312(14) .
O22A C28A 1.385(14) .
O22A C20 1.445(15) .
O31A C39A 1.338(14) .
O32A C38A 1.371(15) .
O32A C30 1.412(15) .
O11B C19B 1.296(15) .
O12B C18B 1.37(2) .
O12B C40 1.43(2) .
O21B C29B 1.335(14) .
O22B C28B 1.377(16) .
O22B C50 1.418(18) .
O31B C18 1.318(14) .
O32B C38B 1.394(14) .
O32B C60 1.457(16) .
O1N N1N 1.191(18) .
O2N N1N 1.226(19) .
O3N N1N 1.241(19) .
O1OX C1OX 1.059(15) .
O1OX C1OX 1.53(2) 3_556
O1OX K2 2.592(11) 3_556
O2OX C1OX 1.27(2) .
N1A C31A 1.464(17) .
N1A C11A 1.486(19) .
N1A C21A 1.493(19) .
N12A C13A 1.302(16) .
N12A C12A 1.441(16) .
N22A C23A 1.273(18) .
N22A C22A 1.485(18) .
N32A C33A 1.269(18) .
N32A C32A 1.486(17) .
N1B C11B 1.483(15) .
N1B C21B 1.497(15) .
N1B C31B 1.507(16) .
N11B C23B 1.271(16) .
N11B C22B 1.495(15) .
N22B C13B 1.308(16) .
N22B C12B 1.445(17) .
N32B C33B 1.298(15) .
N32B C32B 1.472(15) .
C18 C34B 1.392(17) .
C18 C38B 1.418(17) .
C11A C12A 1.53(2) .
C13A C14A 1.430(18) .
C14A C19A 1.388(19) .
C14A C15A 1.416(18) .
C15A C16A 1.35(2) .
C16A C17A 1.40(2) .
C17A C18A 1.390(18) .
C18A C19A 1.452(17) .
C21A C22A 1.556(19) .
C23A C24A 1.43(2) .
C24A C29A 1.419(18) .
C24A C25A 1.425(18) .
C25A C26A 1.35(2) .
C26A C27A 1.43(2) .
C27A C28A 1.374(17) .
C28A C29A 1.431(17) .
C31A C32A 1.51(2) .
C33A C34A 1.44(2) .
C34A C39A 1.394(18) .
C34A C35A 1.454(19) .
C35A C36A 1.37(2) .
C36A C37A 1.37(2) .
C37A C38A 1.386(17) .
C38A C39A 1.417(17) .
C11B C12B 1.524(18) .
C13B C14B 1.45(2) .
C14B C19B 1.39(2) .
C14B C15B 1.429(18) .
C15B C16B 1.37(2) .
C16B C17B 1.35(3) .
C17B C18B 1.37(2) .
C18B C19B 1.440(19) .
C21B C22B 1.481(19) .
C23B C24B 1.477(18) .
C24B C29B 1.400(18) .
C24B C25B 1.413(17) .
C25B C26B 1.34(2) .
C26B C27B 1.37(2) .
C27B C28B 1.408(17) .
C28B C29B 1.390(18) .
C31B C32B 1.508(17) .
C33B C34B 1.445(17) .
C34B C35B 1.421(17) .
C35B C36B 1.372(19) .
C36B C37B 1.382(18) .
C37B C38B 1.397(17) .
C1OX C1OX 1.14(4) 3_556
C1OX O1OX 1.53(2) 3_556
O34 C83 1.39(2) .
