#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:58:55 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179272 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/92/4319217.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_4319217
loop_
_publ_author_name
'F. Albert Cotton'
'Chun Lin'
'Carlos A. Murillo'
_publ_section_title
;
 Supramolecular Squares with Mo24+ Corners
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              478
_journal_page_last               484
_journal_paper_doi               10.1021/ic001016t
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety         '[Mo2(AniF)2]4(C2O4)4(11CH2Cl2)'
_chemical_formula_sum            'C139 H142 Cl22 Mo8 N16 O32'
_chemical_formula_weight         4096.11
_chemical_name_systematic
; 
 ? 
;
_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                 90.70(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   19.089(1)
_cell_length_b                   18.708(1)
_cell_length_c                   23.708(1)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      20.8
_cell_measurement_theta_min      9.0
_cell_volume                     8465.9(7)
_computing_cell_refinement       MADNES
_computing_data_collection       MADNES
_computing_data_reduction        PROCOR
_computing_molecular_graphics    'XP (Siemens, 1990)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.951
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device       'Nonius FAST area detector'
_diffrn_measurement_method       'Ellipsoid-mask fitting'
_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  0.0513
_diffrn_reflns_av_sigmaI/netI    0.0402
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            34342
_diffrn_reflns_theta_full        22.56
_diffrn_reflns_theta_max         22.56
_diffrn_reflns_theta_min         2.29
_diffrn_standards_number         'None (area detector data)'
_exptl_absorpt_coefficient_mu    0.991
_exptl_absorpt_correction_T_max  0.782
_exptl_absorpt_correction_T_min  0.610
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4108
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.119
_refine_diff_density_min         -0.922
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.090
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     960
_refine_ls_number_reflns         10993
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0999
_refine_ls_R_factor_obs          0.0754
_refine_ls_shift/esd_max         0.041
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0595P)²+122.5709P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1943
_refine_ls_wR_factor_obs         0.1723
_reflns_number_total             10993
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic001016t_1.cif
_cod_data_source_block           cmpd_1
_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 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0595P)^2^+122.5709P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0595P)^2^+122.5709P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4319217
#BEGIN Tags that were not found in dictionaries:
_reflns_number_obs               8727
#END Tags that were not found in dictionaries
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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.47960(3) 0.76387(3) -0.47323(2) 0.02821(14) Uani 1 d . . .
Mo2 Mo 0.57992(3) 0.74038(3) -0.44261(2) 0.03020(15) Uani 1 d . . .
Mo3 Mo 0.35566(3) 0.46849(3) -0.32253(2) 0.02916(15) Uani 1 d . . .
Mo4 Mo 0.45770(3) 0.45132(3) -0.29205(2) 0.03007(15) Uani 1 d . . .
N1 N 0.5160(3) 0.8494(3) -0.5232(2) 0.0297(14) Uani 1 d . . .
N2 N 0.6248(3) 0.8272(3) -0.4864(2) 0.0334(14) Uani 1 d . . .
N3 N 0.4556(3) 0.8264(3) -0.4016(2) 0.0325(14) Uani 1 d . . .
N4 N 0.5621(3) 0.7941(3) -0.3653(2) 0.0362(15) Uani 1 d . . .
N5 N 0.3314(3) 0.5378(3) -0.2558(2) 0.0323(14) Uani 1 d . . .
N6 N 0.4424(3) 0.5171(3) -0.2216(2) 0.0348(15) Uani 1 d . . .
N7 N 0.3173(3) 0.3760(3) -0.2819(2) 0.0333(14) Uani 1 d . . .
N8 N 0.4288(3) 0.3575(3) -0.2487(2) 0.0342(15) Uani 1 d . . .
O1 O 0.3253(3) 1.0068(3) -0.6526(3) 0.075(2) Uani 1 d D . .
O2 O 0.9142(3) 0.8597(5) -0.4835(3) 0.098(3) Uani 1 d . . .
O3 O 0.1837(3) 0.9330(5) -0.3893(3) 0.088(2) Uani 1 d D . .
O5 O 0.0686(3) 0.6650(3) -0.2365(2) 0.0667(18) Uani 1 d . . .
O6 O 0.6487(3) 0.5968(4) -0.0663(3) 0.079(2) Uani 1 d . . .
O9 O 0.4921(2) 0.6965(2) -0.54467(18) 0.0328(12) Uani 1 d . . .
O10 O 0.6016(2) 0.6749(2) -0.51367(17) 0.0303(11) Uani 1 d . . .
O11 O 0.4369(2) 0.6742(2) -0.42893(18) 0.0311(11) Uani 1 d . . .
O12 O 0.5454(2) 0.6469(2) -0.40060(18) 0.0301(11) Uani 1 d . . .
O13 O 0.3880(2) 0.5590(2) -0.37120(17) 0.0291(11) Uani 1 d . . .
O14 O 0.4953(2) 0.5405(2) -0.33773(18) 0.0317(11) Uani 1 d . . .
O15 O 0.3739(2) 0.4051(2) -0.39455(18) 0.0312(11) Uani 1 d . . .
O16 O 0.4829(2) 0.3869(2) -0.36356(18) 0.0323(12) Uani 1 d . . .
C1 C 0.5828(4) 0.8641(4) -0.5217(3) 0.0397(19) Uani 1 d . . .
H1A H 0.6013 0.9000 -0.5450 0.048 Uiso 1 calc R . .
C2 C 0.5006(3) 0.8259(3) -0.3596(3) 0.0325(17) Uani 1 d . . .
H2A H 0.4893 0.8481 -0.3253 0.039 Uiso 1 calc R . .
C3 C 0.3811(4) 0.5493(3) -0.2169(3) 0.0344(18) Uani 1 d . . .
H3A H 0.3726 0.5799 -0.1863 0.041 Uiso 1 calc R . .
C4 C 0.3623(3) 0.3368(3) -0.2531(3) 0.0319(17) Uani 1 d . . .
H4A H 0.3475 0.2944 -0.2356 0.038 Uiso 1 calc R . .
C5 C 0.5519(4) 0.6677(3) -0.5489(3) 0.0316(17) Uani 1 d . . .
C6 C 0.4798(3) 0.6362(3) -0.4021(3) 0.0302(17) Uani 1 d . . .
C7 C 0.4515(3) 0.5741(3) -0.3679(3) 0.0281(16) Uani 1 d . . .
C8 C 0.4343(3) 0.3778(3) -0.3993(3) 0.0284(16) Uani 1 d . . .
C11 C 0.4701(3) 0.8905(4) -0.5590(3) 0.0321(17) Uani 1 d . . .
C12 C 0.4762(4) 0.9628(4) -0.5670(3) 0.045(2) Uani 1 d . . .
H12A H 0.5145 0.9874 -0.5511 0.054 Uiso 1 calc R . .
C13 C 0.4269(4) 0.9997(4) -0.5980(3) 0.049(2) Uani 1 d . . .
H13A H 0.4314 1.0494 -0.6022 0.059 Uiso 1 calc R . .
C14 C 0.3709(4) 0.9646(4) -0.6231(3) 0.051(2) Uani 1 d . . .
C15 C 0.3660(4) 0.8921(4) -0.6158(3) 0.047(2) Uani 1 d . . .
H15A H 0.3283 0.8673 -0.6325 0.056 Uiso 1 calc R . .
C16 C 0.4143(4) 0.8554(4) -0.5850(3) 0.041(2) Uani 1 d . . .
H16A H 0.4100 0.8056 -0.5811 0.049 Uiso 1 calc R . .
C17 C 0.2544(7) 0.9867(12) -0.6581(11) 0.068(4) Uiso 0.415(18) d PD A 1
H17A H 0.2293 1.0223 -0.6801 0.103 Uiso 0.415(18) calc PR A 1
H17B H 0.2338 0.9831 -0.6210 0.103 Uiso 0.415(18) calc PR A 1
H17C H 0.2512 0.9407 -0.6769 0.103 Uiso 0.415(18) calc PR A 1
C17' C 0.2694(7) 0.9721(9) -0.6817(7) 0.068(4) Uiso 0.585(18) d PD A 2
H17D H 0.2407 1.0075 -0.7010 0.103 Uiso 0.585(18) calc PR A 2
H17E H 0.2410 0.9461 -0.6550 0.103 Uiso 0.585(18) calc PR A 2
H17F H 0.2883 0.9390 -0.7091 0.103 Uiso 0.585(18) calc PR A 2
C21 C 0.6976(3) 0.8358(4) -0.4885(3) 0.0377(19) Uani 1 d . . .
C22 C 0.7365(5) 0.8181(5) -0.5338(4) 0.068(3) Uani 1 d . . .
H22A H 0.7141 0.8000 -0.5663 0.082 Uiso 1 calc R . .
C23 C 0.8093(4) 0.8262(6) -0.5331(4) 0.076(3) Uani 1 d . . .
H23A H 0.8347 0.8147 -0.5656 0.091 Uiso 1 calc R . .
C24 C 0.8434(4) 0.8497(5) -0.4878(4) 0.067(3) Uani 1 d . . .
C25 C 0.8064(5) 0.8647(7) -0.4397(5) 0.091(4) Uani 1 d . . .
H25A H 0.8302 0.8791 -0.4067 0.109 Uiso 1 calc R . .
C26 C 0.7352(4) 0.8587(6) -0.4401(4) 0.072(3) Uani 1 d . . .
H26A H 0.7105 0.8701 -0.4073 0.086 Uiso 1 calc R . .
C27 C 0.9556(5) 0.8396(7) -0.5292(5) 0.100(4) Uani 1 d . . .
H27A H 1.0044 0.8497 -0.5205 0.149 Uiso 1 calc R . .
H27B H 0.9412 0.8665 -0.5624 0.149 Uiso 1 calc R . .
H27C H 0.9498 0.7889 -0.5364 0.149 Uiso 1 calc R . .
C31 C 0.3881(3) 0.8569(4) -0.3958(3) 0.0362(18) Uani 1 d . . .
C32 C 0.3457(4) 0.8407(6) -0.3526(4) 0.068(3) Uani 1 d . . .
H32A H 0.3616 0.8112 -0.3230 0.082 Uiso 1 calc R . .
C33 C 0.2776(5) 0.8689(7) -0.3526(4) 0.091(4) Uani 1 d . . .
H33A H 0.2488 0.8588 -0.3217 0.110 Uiso 1 calc R . .
C34 C 0.2511(4) 0.9097(5) -0.3949(3) 0.062(3) Uani 1 d . . .
C35 C 0.2945(4) 0.9276(5) -0.4386(4) 0.058(2) Uani 1 d . . .
H35A H 0.2789 0.9576 -0.4680 0.069 Uiso 1 calc R . .
C36 C 0.3618(4) 0.9002(4) -0.4380(3) 0.045(2) Uani 1 d . . .
H36A H 0.3912 0.9117 -0.4681 0.054 Uiso 1 calc R . .
C37 C 0.1602(8) 0.9853(8) -0.4292(6) 0.073(4) Uiso 0.63(2) d PD B 1
H37A H 0.1120 0.9981 -0.4214 0.109 Uiso 0.63(2) calc PR B 1
H37B H 0.1631 0.9658 -0.4670 0.109 Uiso 0.63(2) calc PR B 1
H37C H 0.1895 1.0275 -0.4262 0.109 Uiso 0.63(2) calc PR B 1
C37' C 0.1428(11) 0.9565(15) -0.4343(8) 0.073(4) Uiso 0.37(2) d PD B 2
H37D H 0.0971 0.9706 -0.4209 0.109 Uiso 0.37(2) calc PR B 2
H37E H 0.1375 0.9182 -0.4616 0.109 Uiso 0.37(2) calc PR B 2
H37F H 0.1653 0.9971 -0.4520 0.109 Uiso 0.37(2) calc PR B 2
C41 C 0.6101(8) 0.7906(6) -0.3203(6) 0.0365(17) Uiso 0.389(7) d PD C 1
C42 C 0.6514(7) 0.7298(7) -0.3145(6) 0.048(3) Uiso 0.389(7) d PD C 1
H42 H 0.6457 0.6906 -0.3389 0.057 Uiso 0.389(7) calc PR C 1
C43 C 0.7014(9) 0.7288(8) -0.2713(6) 0.057(3) Uiso 0.389(7) d PD C 1
H43 H 0.7322 0.6897 -0.2685 0.069 Uiso 0.389(7) calc PR C 1
C44 C 0.7074(8) 0.7829(7) -0.2326(6) 0.055(2) Uiso 0.389(7) d PD C 1
C45 C 0.6671(7) 0.8448(7) -0.2401(6) 0.042(2) Uiso 0.389(7) d PD C 1
H45 H 0.6733 0.8840 -0.2158 0.050 Uiso 0.389(7) calc PR C 1
C46 C 0.6178(8) 0.8480(7) -0.2838(6) 0.038(2) Uiso 0.389(7) d PD C 1
H46 H 0.5898 0.8889 -0.2884 0.045 Uiso 0.389(7) calc PR C 1
C47 C 0.8002(9) 0.8085(11) -0.1654(10) 0.075(4) Uiso 0.389(7) d PD C 1
H47A H 0.8196 0.7907 -0.1302 0.112 Uiso 0.389(7) calc PR C 1
H47B H 0.7836 0.8571 -0.1602 0.112 Uiso 0.389(7) calc PR C 1
H47C H 0.8361 0.8080 -0.1940 0.112 Uiso 0.389(7) calc PR C 1
O4 O 0.7425(7) 0.7637(8) -0.1832(5) 0.071(3) Uani 0.389(7) d PD C 1
C41' C 0.6108(6) 0.7860(5) -0.3160(5) 0.0365(17) Uiso 0.611(7) d PD C 2
C42' C 0.6273(6) 0.7173(6) -0.2982(5) 0.048(3) Uiso 0.611(7) d PD C 2
H42' H 0.6063 0.6771 -0.3153 0.057 Uiso 0.611(7) calc PR C 2
C43' C 0.6758(6) 0.7098(6) -0.2544(5) 0.057(3) Uiso 0.611(7) d PD C 2
H43' H 0.6870 0.6634 -0.2420 0.069 Uiso 0.611(7) calc PR C 2
C44' C 0.7076(6) 0.7655(6) -0.2287(5) 0.055(2) Uiso 0.611(7) d PD C 2
C45' C 0.6901(6) 0.8343(5) -0.2465(4) 0.042(2) Uiso 0.611(7) d PD C 2
H45' H 0.7112 0.8740 -0.2289 0.050 Uiso 0.611(7) calc PR C 2
C46' C 0.6416(6) 0.8445(5) -0.2899(4) 0.038(2) Uiso 0.611(7) d PD C 2
H46' H 0.6298 0.8910 -0.3016 0.045 Uiso 0.611(7) calc PR C 2
C47' C 0.7765(9) 0.8165(8) -0.1544(6) 0.075(4) Uiso 0.611(7) d PD C 2
H47D H 0.8160 0.8065 -0.1295 0.112 Uiso 0.611(7) calc PR C 2
H47E H 0.7351 0.8252 -0.1321 0.112 Uiso 0.611(7) calc PR C 2
H47F H 0.7866 0.8585 -0.1770 0.112 Uiso 0.611(7) calc PR C 2
O4' O 0.7641(5) 0.7552(6) -0.1917(4) 0.071(3) Uani 0.611(7) d PD C 2
C51 C 0.2650(3) 0.5703(3) -0.2470(3) 0.0329(17) Uani 1 d . . .
C52 C 0.2324(4) 0.6053(4) -0.2932(3) 0.0395(19) Uani 1 d . . .
H52A H 0.2553 0.6075 -0.3280 0.047 Uiso 1 calc R . .
C53 C 0.1687(4) 0.6354(4) -0.2876(3) 0.045(2) Uani 1 d . . .
H53A H 0.1479 0.6590 -0.3185 0.054 Uiso 1 calc R . .
C54 C 0.1337(4) 0.6321(4) -0.2371(3) 0.046(2) Uani 1 d . . .
C55 C 0.1643(4) 0.5980(4) -0.1917(3) 0.045(2) Uani 1 d . . .
H55A H 0.1407 0.5958 -0.1572 0.054 Uiso 1 calc R . .
C56 C 0.2298(4) 0.5669(4) -0.1968(3) 0.046(2) Uani 1 d . . .
H56A H 0.2503 0.5433 -0.1657 0.055 Uiso 1 calc R . .
C57 C 0.0320(5) 0.6650(7) -0.1841(4) 0.099(4) Uani 1 d . . .
H57A H -0.0125 0.6893 -0.1889 0.148 Uiso 1 calc R . .
H57B H 0.0600 0.6896 -0.1557 0.148 Uiso 1 calc R . .
H57C H 0.0239 0.6161 -0.1722 0.148 Uiso 1 calc R . .
C61 C 0.4962(3) 0.5384(4) -0.1824(3) 0.0359(18) Uani 1 d . . .
C62 C 0.5231(4) 0.6066(4) -0.1832(4) 0.056(2) Uani 1 d . . .
H62A H 0.5062 0.6396 -0.2101 0.068 Uiso 1 calc R . .
C63 C 0.5743(4) 0.6275(4) -0.1454(4) 0.060(3) Uani 1 d . . .
H63A H 0.5922 0.6743 -0.1467 0.072 Uiso 1 calc R . .
C64 C 0.5990(4) 0.5806(4) -0.1061(3) 0.051(2) Uani 1 d . . .
C65 C 0.5724(5) 0.5131(5) -0.1050(4) 0.064(3) Uani 1 d . . .
H65A H 0.5895 0.4802 -0.0782 0.077 Uiso 1 calc R . .
C66 C 0.5215(5) 0.4925(4) -0.1423(3) 0.055(2) Uani 1 d . . .
H66A H 0.5034 0.4458 -0.1404 0.066 Uiso 1 calc R . .
C67 C 0.6754(5) 0.6661(6) -0.0613(5) 0.087(4) Uani 1 d . . .
H67A H 0.7101 0.6676 -0.0311 0.130 Uiso 1 calc R . .
H67B H 0.6376 0.6990 -0.0529 0.130 Uiso 1 calc R . .
H67C H 0.6970 0.6800 -0.0965 0.130 Uiso 1 calc R . .
C71 C 0.2500(3) 0.3481(3) -0.2921(3) 0.0325(17) Uani 1 d . . .
C72 C 0.1929(4) 0.3943(4) -0.2913(3) 0.045(2) Uani 1 d . . .
H72A H 0.2005 0.4426 -0.2823 0.054 Uiso 1 calc R . .
C73 C 0.1248(4) 0.3716(4) -0.3034(4) 0.055(2) Uani 1 d . . .
H73A H 0.0874 0.4042 -0.3040 0.066 Uiso 1 calc R . .
C74 C 0.1136(4) 0.2998(5) -0.3145(4) 0.061(3) Uani 1 d . . .
C75 C 0.1678(5) 0.2540(5) -0.3146(5) 0.083(4) Uani 1 d . . .
H75A H 0.1597 0.2055 -0.3228 0.100 Uiso 1 calc R . .
C76 C 0.2369(5) 0.2772(4) -0.3027(4) 0.068(3) Uani 1 d . . .
H76A H 0.2738 0.2440 -0.3019 0.081 Uiso 1 calc R . .
C77 C 0.0078(11) 0.3010(15) -0.3481(17) 0.082(4) Uiso 0.262(14) d PD D 1
H77A H -0.0319 0.2732 -0.3614 0.123 Uiso 0.262(14) calc PR D 1
H77B H 0.0237 0.3322 -0.3780 0.123 Uiso 0.262(14) calc PR D 1
H77C H -0.0059 0.3296 -0.3160 0.123 Uiso 0.262(14) calc PR D 1
O7 O 0.0608(12) 0.2560(12) -0.3324(15) 0.093(3) Uani 0.262(14) d PD D 1
C77' C -0.0098(7) 0.3207(8) -0.3265(6) 0.082(4) Uiso 0.738(14) d PD D 2
H77D H -0.0529 0.2942 -0.3328 0.123 Uiso 0.738(14) calc PR D 2
H77E H -0.0028 0.3538 -0.3574 0.123 Uiso 0.738(14) calc PR D 2
H77F H -0.0129 0.3471 -0.2914 0.123 Uiso 0.738(14) calc PR D 2
O7' O 0.0451(5) 0.2744(5) -0.3234(6) 0.093(3) Uani 0.738(14) d PD D 2
C81 C 0.4763(4) 0.3190(4) -0.2131(3) 0.0387(19) Uani 1 d . . .
C82 C 0.5434(4) 0.3067(4) -0.2315(3) 0.052(2) Uani 1 d . . .
H82A H 0.5563 0.3228 -0.2675 0.063 Uiso 1 calc R . .
C83 C 0.5918(5) 0.2713(5) -0.1983(5) 0.075(3) Uani 1 d . . .
H83A H 0.6374 0.2639 -0.2116 0.090 Uiso 1 calc R . .
C84 C 0.5741(5) 0.2473(6) -0.1472(5) 0.083(3) Uani 1 d . . .
C85 C 0.5077(6) 0.2599(5) -0.1280(4) 0.077(3) Uani 1 d . . .
H85A H 0.4958 0.2431 -0.0920 0.093 Uiso 1 calc R . .
C86 C 0.4573(5) 0.2965(4) -0.1596(3) 0.056(2) Uani 1 d . . .
H86A H 0.4124 0.3055 -0.1454 0.067 Uiso 1 calc R . .
C87 C 0.6924(8) 0.1916(14) -0.1403(11) 0.115(6) Uiso 0.520(11) d PD E 1
H87A H 0.7176 0.1630 -0.1126 0.173 Uiso 0.520(11) calc PR E 1
H87B H 0.7180 0.2355 -0.1471 0.173 Uiso 0.520(11) calc PR E 1
H87C H 0.6877 0.1649 -0.1752 0.173 Uiso 0.520(11) calc PR E 1
O8 O 0.6263(6) 0.2079(8) -0.1200(5) 0.077(3) Uani 0.520(11) d PD E 1
C87' C 0.6752(9) 0.2074(17) -0.1147(13) 0.115(6) Uiso 0.480(11) d PD E 2
H87D H 0.7028 0.1845 -0.0852 0.173 Uiso 0.480(11) calc PR E 2
H87E H 0.6934 0.2550 -0.1215 0.173 Uiso 0.480(11) calc PR E 2
H87F H 0.6778 0.1794 -0.1490 0.173 Uiso 0.480(11) calc PR E 2
O8' O 0.6060(7) 0.2122(9) -0.0980(6) 0.077(3) Uani 0.480(11) d PD E 2
C1S C -0.0886(9) 0.4366(8) -0.4826(7) 0.143(6) Uiso 1 d D . .
Cl1 Cl -0.1347(6) 0.4439(7) -0.4198(4) 0.177(4) Uiso 0.509(10) d PD F 1
Cl1' Cl -0.1402(6) 0.3982(8) -0.4284(5) 0.198(5) Uiso 0.491(10) d PD F 2
Cl2 Cl -0.0288(3) 0.3717(4) -0.4892(3) 0.208(2) Uiso 1 d . . .
C2S C 0.2814(6) 0.6932(8) -0.4388(5) 0.060(3) Uiso 0.600(7) d PD G 1
Cl3 Cl 0.1898(2) 0.7001(3) -0.4373(2) 0.0912(7) Uani 0.600(7) d PD G 1
Cl4 Cl 0.3111(3) 0.7262(3) -0.5056(2) 0.0912(7) Uani 0.600(7) d PD G 1
C2S' C 0.2814(7) 0.6622(9) -0.4560(7) 0.060(3) Uiso 0.400(7) d PD G 2
Cl3' Cl 0.2006(4) 0.6864(5) -0.4281(3) 0.0912(7) Uani 0.400(7) d PD G 2
Cl4' Cl 0.3103(4) 0.7272(6) -0.5061(4) 0.0912(7) Uani 0.400(7) d PD G 2
C3S C 0.7259(6) 0.1060(6) 0.0570(5) 0.082(3) Uiso 1 d . . .
Cl5 Cl 0.72235(14) 0.01492(15) 0.08104(12) 0.0844(8) Uani 1 d . . .
Cl6 Cl 0.6562(2) 0.1259(3) 0.0145(2) 0.189(2) Uani 1 d . . .
C4S C 0.4711(5) 0.9265(8) -0.8316(4) 0.123(5) Uiso 1 d D . .
Cl7 Cl 0.4258(4) 0.9737(4) -0.7813(3) 0.199(3) Uani 0.735(9) d PD H 1
Cl7' Cl 0.4690(12) 0.9813(10) -0.7714(7) 0.199(3) Uani 0.265(9) d PD H 2
Cl8 Cl 0.5350(3) 0.9725(2) -0.8684(2) 0.1463(17) Uani 1 d D . .
C6S C 0.4168(5) 0.5454(10) -0.5357(10) 0.148(7) Uiso 0.50 d PD . 1
Cl11 Cl 0.4898(5) 0.5027(7) -0.5025(5) 0.0948(15) Uani 0.50 d PD . 1
Cl12 Cl 0.3369(5) 0.4988(5) -0.5504(4) 0.0948(15) Uani 0.279(5) d PD I 1
Cl13 Cl 0.3323(6) 0.5170(7) -0.5211(6) 0.0948(15) Uani 0.221(5) d PD I 1
C5S C 0.8474(2) 1.0348(2) -0.2046(2) 0.148(7) Uiso 0.56(2) d PG . 2
Cl18 Cl 0.2360(3) 0.9631(3) -0.8210(2) 0.1067(12) Uani 0.496(3) d PG . 2
Cl19 Cl 0.1240(2) 0.0413(3) 0.2312(2) 0.1067(12) Uani 0.713(3) d PG . 2
C7S C 0.3639(4) 0.5029(5) -0.6120(4) 0.148(7) Uiso 0.44(2) d PG . 3
Cl14 Cl 0.3635(4) 0.5606(5) -0.5520(4) 0.1067(12) Uani 0.2183(10) d PG J 3
Cl15 Cl 0.8436(7) 0.9957(8) -0.1905(6) 0.1067(12) Uani 0.2322(14) d PG . 3
Cl16 Cl 0.2075(7) 0.9758(6) -0.8455(5) 0.1067(12) Uani 0.1986(19) d PG . 3
Cl17 Cl 0.2912(4) 0.4991(5) -0.5838(4) 0.1067(12) Uani 0.142(2) d PG . 3
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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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
Mo2 Mo1 N1 92.73(14) . . y
Mo2 Mo1 N3 92.50(15) . . y
N1 Mo1 N3 96.2(2) . . y
Mo2 Mo1 O9 92.34(12) . . y
N1 Mo1 O9 87.74(18) . . y
N3 Mo1 O9 173.62(19) . . y
Mo2 Mo1 O11 91.02(11) . . y
N1 Mo1 O11 174.80(18) . . y
N3 Mo1 O11 87.25(18) . . y
O9 Mo1 O11 88.51(16) . . y
Mo1 Mo2 N2 92.50(15) . . y
Mo1 Mo2 O12 92.74(11) . . y
N2 Mo2 O12 173.55(18) . . y
Mo1 Mo2 N4 92.56(15) . . y
N2 Mo2 N4 97.5(2) . . y
O12 Mo2 N4 86.00(19) . . y
Mo1 Mo2 O10 91.84(12) . . y
N2 Mo2 O10 88.28(18) . . y
O12 Mo2 O10 87.80(16) . . y
N4 Mo2 O10 172.56(19) . . y
Mo4 Mo3 N5 92.72(15) . . y
Mo4 Mo3 O15 91.75(12) . . y
N5 Mo3 O15 174.52(18) . . y
Mo4 Mo3 N7 92.44(15) . . y
N5 Mo3 N7 94.7(2) . . y
O15 Mo3 N7 88.31(18) . . y
Mo4 Mo3 O13 91.93(11) . . y
N5 Mo3 O13 89.15(18) . . y
O15 Mo3 O13 87.53(16) . . y
N7 Mo3 O13 174.05(18) . . y
Mo3 Mo4 N6 92.69(15) . . y
Mo3 Mo4 N8 92.77(16) . . y
N6 Mo4 N8 93.5(2) . . y
Mo3 Mo4 O14 91.30(12) . . y
N6 Mo4 O14 89.77(19) . . y
N8 Mo4 O14 174.64(19) . . y
Mo3 Mo4 O16 91.71(12) . . y
N6 Mo4 O16 174.90(19) . . y
N8 Mo4 O16 88.84(18) . . y
O14 Mo4 O16 87.55(17) . . y
C1 N1 C11 119.5(5) . . ?
C1 N1 Mo1 118.2(4) . . ?
C11 N1 Mo1 122.3(4) . . ?
C1 N2 C21 120.2(6) . . ?
C1 N2 Mo2 117.3(4) . . ?
C21 N2 Mo2 121.0(4) . . ?
C2 N3 C31 121.3(6) . . ?
C2 N3 Mo1 117.4(4) . . ?
C31 N3 Mo1 120.4(4) . . ?
C2 N4 C41 121.1(8) . . ?
C2 N4 C41' 120.7(7) . . ?
C2 N4 Mo2 116.9(4) . . ?
C41 N4 Mo2 121.8(7) . . ?
C41' N4 Mo2 121.6(5) . . ?
C3 N5 C51 117.2(5) . . ?
C3 N5 Mo3 117.3(4) . . ?
C51 N5 Mo3 125.4(4) . . ?
C3 N6 C61 116.6(6) . . ?
C3 N6 Mo4 117.8(4) . . ?
C61 N6 Mo4 125.0(4) . . ?
C4 N7 C71 118.3(5) . . ?
C4 N7 Mo3 117.7(4) . . ?
C71 N7 Mo3 123.0(4) . . ?
C4 N8 C81 119.9(6) . . ?
C4 N8 Mo4 117.3(4) . . ?
C81 N8 Mo4 122.7(4) . . ?
C14 O1 C17 120.0(11) . . ?
C14 O1 C17' 117.2(9) . . ?
C24 O2 C27 118.2(8) . . ?
C34 O3 C37' 123.3(11) . . ?
C34 O3 C37 116.3(9) . . ?
C54 O5 C57 117.0(7) . . ?
C64 O6 C67 121.0(8) . . ?
C5 O9 Mo1 115.2(4) . . ?
C5 O10 Mo2 115.7(4) . . ?
C6 O11 Mo1 116.3(4) . . ?
C6 O12 Mo2 115.5(4) . . ?
C7 O13 Mo3 115.6(4) . . ?
C7 O14 Mo4 117.1(4) . . ?
C8 O15 Mo3 117.3(4) . . ?
C8 O16 Mo4 116.0(4) . . ?
N1 C1 N2 119.0(6) . . ?
N3 C2 N4 120.1(6) . . ?
N6 C3 N5 119.5(6) . . ?
N7 C4 N8 119.7(6) . . ?
O10 C5 O9 124.8(6) . . ?
O10 C5 C8 117.2(6) . 3_664 ?
O9 C5 C8 117.9(6) . 3_664 ?
O11 C6 O12 124.2(6) . . ?
O11 C6 C7 118.1(5) . . ?
O12 C6 C7 117.7(5) . . ?
O13 C7 O14 124.0(6) . . ?
O13 C7 C6 119.5(5) . . ?
O14 C7 C6 116.5(5) . . ?
O16 C8 O15 123.2(6) . . ?
O16 C8 C5 119.1(5) . 3_664 ?
O15 C8 C5 117.7(5) . 3_664 ?
C12 C11 C16 118.0(6) . . ?
C12 C11 N1 124.0(6) . . ?
C16 C11 N1 117.9(6) . . ?
C11 C12 C13 120.8(7) . . ?
C12 C13 C14 120.8(7) . . ?
O1 C14 C15 126.4(7) . . ?
O1 C14 C13 115.7(7) . . ?
C15 C14 C13 117.9(7) . . ?
C16 C15 C14 121.5(7) . . ?
C15 C16 C11 120.8(7) . . ?
C22 C21 N2 123.7(7) . . ?
C22 C21 C26 116.1(7) . . ?
N2 C21 C26 120.0(7) . . ?
C21 C22 C23 121.2(8) . . ?
C24 C23 C22 121.6(9) . . ?
C23 C24 O2 125.6(9) . . ?
C23 C24 C25 119.1(8) . . ?
O2 C24 C25 115.3(9) . . ?
C26 C25 C24 119.9(9) . . ?
C25 C26 C21 121.8(9) . . ?
C32 C31 C36 117.9(7) . . ?
C32 C31 N3 122.5(7) . . ?
C36 C31 N3 119.4(6) . . ?
C31 C32 C33 118.7(8) . . ?
C34 C33 C32 123.4(8) . . ?
C33 C34 O3 116.9(8) . . ?
C33 C34 C35 118.2(8) . . ?
O3 C34 C35 124.8(8) . . ?
C34 C35 C36 118.0(8) . . ?
C31 C36 C35 123.8(7) . . ?
C46 C41 C42 121.0(12) . . ?
C46 C41 N4 120.3(10) . . ?
C42 C41 N4 118.6(10) . . ?
C41 C42 C43 117.8(12) . . ?
C44 C43 C42 122.3(13) . . ?
C43 C44 O4 114.1(12) . . ?
C43 C44 C45 119.0(12) . . ?
O4 C44 C45 125.4(12) . . ?
C46 C45 C44 119.7(12) . . ?
C41 C46 C45 119.9(12) . . ?
C44 O4 C47 116.9(14) . . ?
C46' C41' C42' 120.2(10) . . ?
C46' C41' N4 121.9(8) . . ?
C42' C41' N4 117.9(8) . . ?
C41' C42' C43' 117.8(10) . . ?
C44' C43' C42' 123.6(11) . . ?
C43' C44' C45' 118.1(10) . . ?
C43' C44' O4' 121.2(10) . . ?
C45' C44' O4' 119.9(10) . . ?
C46' C45' C44' 120.5(9) . . ?
C41' C46' C45' 119.9(9) . . ?
C44' O4' C47' 112.9(10) . . ?
C56 C51 C52 118.5(6) . . ?
C56 C51 N5 123.6(6) . . ?
C52 C51 N5 117.8(6) . . ?
C53 C52 C51 120.4(7) . . ?
C52 C53 C54 120.9(7) . . ?
C55 C54 C53 119.6(7) . . ?
C55 C54 O5 124.8(7) . . ?
C53 C54 O5 115.6(7) . . ?
C54 C55 C56 120.2(7) . . ?
C51 C56 C55 120.4(7) . . ?
C66 C61 C62 117.6(7) . . ?
C66 C61 N6 121.5(6) . . ?
C62 C61 N6 120.8(6) . . ?
C63 C62 C61 121.1(8) . . ?
C64 C63 C62 120.1(8) . . ?
C63 C64 C65 119.0(8) . . ?
C63 C64 O6 124.3(8) . . ?
C65 C64 O6 116.7(8) . . ?
C66 C65 C64 120.9(8) . . ?
C65 C66 C61 121.2(8) . . ?
C76 C71 C72 117.5(7) . . ?
C76 C71 N7 123.7(7) . . ?
C72 C71 N7 118.9(6) . . ?
C71 C72 C73 122.5(7) . . ?
C74 C73 C72 118.4(7) . . ?
C75 C74 O7 100.5(12) . . ?
C75 C74 C73 120.2(8) . . ?
O7 C74 C73 138.9(12) . . ?
C75 C74 O7' 119.9(8) . . ?
C73 C74 O7' 119.9(8) . . ?
C74 C75 C76 121.3(8) . . ?
C71 C76 C75 120.1(8) . . ?
C74 O7 C77 105(2) . . ?
C77' O7' C74 120.5(10) . . ?
C82 C81 C86 119.6(7) . . ?
C82 C81 N8 118.8(6) . . ?
C86 C81 N8 121.5(7) . . ?
C83 C82 C81 121.2(8) . . ?
C84 C83 C82 120.2(9) . . ?
C83 C84 C85 119.2(9) . . ?
C83 C84 O8 114.1(10) . . ?
C85 C84 O8 126.6(10) . . ?
C83 C84 O8' 139.8(10) . . ?
C85 C84 O8' 100.9(10) . . ?
C84 C85 C86 122.7(9) . . ?
C81 C86 C85 117.0(9) . . ?
C87 O8 C84 127.2(15) . . ?
C87' O8' C84 100.9(16) . . ?
Cl2 C1S Cl1 119.2(11) . . ?
Cl2 C1S Cl1' 99.1(10) . . ?
Cl3 C2S Cl4 108.6(6) . . ?
Cl3' C2S' Cl4' 110.8(9) . . ?
Cl6 C3S Cl5 111.2(6) . . ?
Cl7 C4S Cl8 117.0(9) . . ?
Cl8 C4S Cl7' 98.2(10) . . ?
Cl13 C6S Cl11 119.8(12) . . ?
Cl11 C6S Cl12 121.8(12) . . ?
Cl13 C6S Cl11 123.1(12) . 3_664 ?
Cl12 C6S Cl11 124.8(11) . 3_664 ?
Cl19 C5S Cl18 117.9(5) 3_665 3_674 ?
Cl16 C7S Cl14 128.3(5) 2_543 . ?
Cl17 C7S Cl15 104.5 . 4_575 ?
Cl14 C7S Cl15 140.4(6) . 4_575 ?
Cl15 Cl16 Cl17 120.7(10) 3_674 2_553 ?
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
Mo1 Mo2 2.0865(8) . y
Mo1 N1 2.114(5) . y
Mo1 N3 2.117(5) . y
Mo1 O9 2.127(4) . y
Mo1 O11 2.145(4) . y
Mo2 N2 2.114(5) . y
Mo2 O12 2.121(4) . y
Mo2 N4 2.121(6) . y
Mo2 O10 2.128(4) . y
Mo3 Mo4 2.0940(8) . y
Mo3 N5 2.101(5) . y
Mo3 O15 2.112(4) . y
Mo3 N7 2.116(5) . y
Mo3 O13 2.144(4) . y
Mo4 N6 2.098(5) . y
Mo4 N8 2.111(5) . y
Mo4 O14 2.119(4) . y
Mo4 O16 2.139(4) . y
N1 C1 1.305(9) . ?
N1 C11 1.436(8) . ?
N2 C1 1.344(9) . ?
N2 C21 1.400(9) . ?
N3 C2 1.306(8) . ?
N3 C31 1.418(8) . ?
N4 C2 1.324(9) . ?
N4 C41 1.399(14) . ?
N4 C41' 1.492(12) . ?
N5 C3 1.333(9) . ?
N5 C51 1.424(8) . ?
N6 C3 1.322(9) . ?
N6 C61 1.433(9) . ?
N7 C4 1.313(8) . ?
N7 C71 1.405(8) . ?
N8 C4 1.330(8) . ?
N8 C81 1.427(9) . ?
O1 C14 1.363(10) . ?
O1 C17 1.409(14) . ?
O1 C17' 1.421(14) . ?
O2 C24 1.366(10) . ?
O2 C27 1.401(13) . ?
O3 C34 1.367(10) . ?
O3 C37' 1.386(17) . ?
O3 C37 1.429(14) . ?
O5 C54 1.388(9) . ?
O5 C57 1.433(11) . ?
O6 C64 1.364(10) . ?
O6 C67 1.399(12) . ?
O9 C5 1.267(8) . ?
O10 C5 1.264(8) . ?
O11 C6 1.253(7) . ?
O12 C6 1.269(7) . ?
O13 C7 1.245(7) . ?
O14 C7 1.264(7) . ?
O15 C8 1.267(7) . ?
O16 C8 1.260(7) . ?
C5 C8 1.519(9) 3_664 ?
C6 C7 1.518(9) . ?
C8 C5 1.519(9) 3_664 ?
C11 C12 1.371(10) . ?
C11 C16 1.388(10) . ?
C12 C13 1.371(11) . ?
C13 C14 1.382(11) . ?
C14 C15 1.371(11) . ?
C15 C16 1.355(10) . ?
C21 C22 1.353(11) . ?
C21 C26 1.413(11) . ?
C22 C23 1.400(12) . ?
C23 C24 1.324(13) . ?
C24 C25 1.378(14) . ?
C25 C26 1.363(13) . ?
C31 C32 1.347(11) . ?
C31 C36 1.376(10) . ?
C32 C33 1.404(12) . ?
C33 C34 1.352(13) . ?
C34 C35 1.376(12) . ?
C35 C36 1.383(11) . ?
C41 C46 1.386(15) . ?
C41 C42 1.391(15) . ?
C42 C43 1.393(16) . ?
C43 C44 1.369(16) . ?
C44 O4 1.391(14) . ?
C44 C45 1.400(15) . ?
C45 C46 1.391(15) . ?
C47 O4 1.443(17) . ?
C41' C46' 1.384(12) . ?
C41' C42' 1.389(13) . ?
C42' C43' 1.392(14) . ?
C43' C44' 1.347(14) . ?
C44' C45' 1.394(13) . ?
C44' O4' 1.395(12) . ?
C45' C46' 1.389(13) . ?
C47' O4' 1.466(14) . ?
C51 C56 1.375(10) . ?
C51 C52 1.414(10) . ?
C52 C53 1.349(10) . ?
C53 C54 1.381(10) . ?
C54 C55 1.374(10) . ?
C55 C56 1.386(10) . ?
C61 C66 1.365(10) . ?
C61 C62 1.377(11) . ?
C62 C63 1.374(12) . ?
C63 C64 1.360(12) . ?
C64 C65 1.362(12) . ?
C65 C66 1.360(12) . ?
C71 C76 1.374(10) . ?
C71 C72 1.391(10) . ?
C72 C73 1.393(11) . ?
C73 C74 1.384(12) . ?
C74 C75 1.344(13) . ?
C74 O7 1.36(3) . ?
C74 O7' 1.405(12) . ?
C75 C76 1.413(13) . ?
C77 O7 1.36(2) . ?
C77' O7' 1.362(14) . ?
C81 C82 1.377(11) . ?
C81 C86 1.387(11) . ?
C82 C83 1.376(12) . ?
C83 C84 1.340(15) . ?
C84 C85 1.371(15) . ?
C84 O8 1.392(15) . ?
C84 O8' 1.466(17) . ?
C85 C86 1.394(13) . ?
C87 O8 1.388(18) . ?
C87' O8' 1.386(19) . ?
C1S Cl2 1.675(17) . ?
C1S Cl1 1.744(19) . ?
C1S Cl1' 1.780(19) . ?
C2S Cl3 1.754(11) . ?
C2S Cl4 1.798(12) . ?
C2S' Cl3' 1.744(14) . ?
C2S' Cl4' 1.791(15) . ?
C3S Cl6 1.700(11) . ?
C3S Cl5 1.799(11) . ?
C4S Cl7 1.725(12) . ?
C4S Cl8 1.737(11) . ?
C4S Cl7' 1.758(16) . ?
C6S Cl13 1.738(14) . ?
C6S Cl11 1.781(15) . ?
C6S Cl12 1.787(14) . ?
C5S Cl19 1.652(10) 3_665 ?
C5S Cl18 1.713(8) 3_674 ?
Cl18 C5S 1.712(9) 3_674 ?
Cl19 C5S 1.653(9) 3_665 ?
C7S Cl17 1.5503 . ?
C7S Cl16 1.759(17) 2_543 ?
C7S Cl14 1.7852 . ?
C7S Cl15 1.8967 4_575 ?
Cl15 C7S 1.897(12) 4_676 ?
Cl16 C7S 1.759(16) 2_553 ?
