#------------------------------------------------------------------------------
#$Date: 2016-03-21 17:25:37 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178782 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/36/4103667.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_4103667
loop_
_publ_author_name
'Jian-Rong Li'
'Andrey A. Yakovenko'
'Weigang Lu'
'Daren J. Timmons'
'Wenjuan Zhuang'
'Daqiang Yuan'
'Hong-Cai Zhou'
_publ_contact_author
; 
Hong-Cai Zhou
Department of Chemistry, Texas A&M University, 
PO Box 30012, College Station, TX 77842-3012, USA
;
_publ_contact_author_email       zhou@mail.chem.tamu.edu
_publ_section_title
;
 Ligand Bridging-Angle-Driven Assembly of Molecular Architectures Based on
 Quadruply Bonded Mo-Mo Dimers
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17599
_journal_page_last               17610
_journal_paper_doi               10.1021/ja1080794
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C156 H96 Mo6 O42'
_chemical_formula_sum            'C156 H96 Mo6 O42'
_chemical_formula_weight         3217.97
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           176
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   25.807(2)
_cell_length_b                   25.807(2)
_cell_length_c                   29.780(5)
_cell_measurement_reflns_used    3605
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      13.81
_cell_measurement_theta_min      2.25
_cell_volume                     17176(3)
_computing_cell_refinement       'SAINT+ ver. (Bruker, 2001)'
_computing_data_collection       'APEX2  (Bruker, 2008)'
_computing_data_reduction        'SAINT+ ver. (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.2653
_diffrn_reflns_av_sigmaI/netI    0.2805
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            151822
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.58
_exptl_absorpt_coefficient_mu    0.247
_exptl_absorpt_correction_T_max  0.9569
_exptl_absorpt_correction_T_min  0.9522
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    0.622
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3240
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_platon_squeeze_details
;
;
_refine_diff_density_max         0.677
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         10274
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.3540
_refine_ls_R_factor_gt           0.0975
_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)+(0.0300P)²+15.5000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1645
_refine_ls_wR_factor_ref         0.1997
_reflns_number_gt                2576
_reflns_number_total             10274
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ja1080794_si_002_07.cif
_cod_data_source_block           2C
_cod_depositor_comments
;
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 
;
_cod_original_cell_volume        17176(4)
_cod_database_code               4103667
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -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
Mo1 Mo 0.13895(5) 0.34375(6) 0.2500 0.1114(5) Uani 1 2 d SD
Mo2 Mo 0.19434(5) 0.43742(5) 0.2500 0.1038(5) Uani 1 2 d SD
O1 O 0.1922(2) 0.3340(2) 0.29869(16) 0.1092(19) Uani 1 1 d D
O2 O 0.2502(2) 0.4341(2) 0.29737(17) 0.1033(19) Uani 1 1 d D
O3 O 0.6530(3) 0.7351(3) 0.2989(2) 0.118(2) Uani 1 1 d .
O4 O 0.5526(3) 0.6944(3) 0.29832(19) 0.105(2) Uani 1 1 d .
O5 O 0.6027(3) 0.3805(3) 0.5834(2) 0.168(3) Uani 1 1 d .
O6 O 0.4956(3) 0.2946(3) 0.5878(2) 0.143(2) Uani 1 1 d .
O8 O 0.2476(3) 0.54493(7) 0.2500 0.202(5) Uani 1 2 d SD
O7 O 0.0751(3) 0.23700(8) 0.2500 0.201(4) Uani 1 2 d SD
C1 C 0.23598(18) 0.3827(2) 0.31276(15) 0.104(3) Uani 1 1 d D
C2 C 0.27704(14) 0.37898(16) 0.34682(12) 0.1504(17) Uani 1 1 d GD
C3 C 0.2661(2) 0.32352(17) 0.36215(17) 0.1504(17) Uani 1 1 d GD
H3A H 0.2326 0.2880 0.3511 0.181 Uiso 1 1 calc R
C4 C 0.3040(3) 0.3201(2) 0.39361(17) 0.1504(17) Uani 1 1 d GD
H4A H 0.2965 0.2822 0.4041 0.181 Uiso 1 1 calc R
C5 C 0.3530(2) 0.3721(3) 0.40975(13) 0.1504(17) Uani 1 1 d GD
C6 C 0.36392(19) 0.4276(2) 0.39441(16) 0.1504(17) Uani 1 1 d GD
H6A H 0.3973 0.4631 0.4054 0.181 Uiso 1 1 calc R
C7 C 0.32596(18) 0.43101(17) 0.36295(16) 0.1504(17) Uani 1 1 d GD
H7A H 0.3335 0.4689 0.3525 0.181 Uiso 1 1 calc R
C8 C 0.3972(4) 0.3752(5) 0.4433(3) 0.158(3) Uani 1 1 d D
C9 C 0.4330(3) 0.3774(5) 0.4677(3) 0.158(3) Uani 1 1 d D
C10 C 0.4787(3) 0.3813(3) 0.49619(17) 0.1335(14) Uani 1 1 d GD
C11 C 0.4637(2) 0.3350(2) 0.5265(2) 0.1335(14) Uani 1 1 d GD
H11A H 0.4240 0.3022 0.5276 0.160 Uiso 1 1 calc R
C12 C 0.5070(3) 0.3368(2) 0.55531(17) 0.1335(14) Uani 1 1 d GD
C13 C 0.5651(3) 0.3848(3) 0.55377(18) 0.1335(14) Uani 1 1 d GD
C14 C 0.5801(2) 0.4311(2) 0.5234(2) 0.1335(14) Uani 1 1 d GD
H14A H 0.6198 0.4639 0.5224 0.160 Uiso 1 1 calc R
C15 C 0.5368(3) 0.4294(2) 0.49465(16) 0.1335(14) Uani 1 1 d GD
C16 C 0.5553(4) 0.4783(4) 0.4644(3) 0.1335(14) Uani 1 1 d D
C17 C 0.5666(3) 0.5184(4) 0.4379(3) 0.1335(14) Uani 1 1 d D
C18 C 0.5805(6) 0.5647(4) 0.40707(18) 0.140(4) Uani 1 1 d GD
C19 C 0.6373(4) 0.6087(5) 0.3939(3) 0.193(6) Uani 1 1 d GD
H19A H 0.6716 0.6093 0.4061 0.231 Uiso 1 1 calc R
C20 C 0.6440(4) 0.6519(4) 0.3629(3) 0.148(4) Uani 1 1 d GD
H20A H 0.6829 0.6820 0.3539 0.178 Uiso 1 1 calc R
C21 C 0.5938(6) 0.6509(3) 0.34498(17) 0.117(3) Uani 1 1 d GD
C22 C 0.5369(4) 0.6069(5) 0.3581(3) 0.137(4) Uani 1 1 d GD
H22A H 0.5026 0.6063 0.3459 0.165 Uiso 1 1 calc R
C23 C 0.5303(4) 0.5638(3) 0.3892(3) 0.160(5) Uani 1 1 d GD
H23A H 0.4914 0.5336 0.3982 0.192 Uiso 1 1 calc R
C24 C 0.5994(6) 0.6972(4) 0.3111(3) 0.093(3) Uani 1 1 d D
C25 C 0.6631(5) 0.4225(5) 0.5792(4) 0.202(6) Uani 1 1 d .
H25A H 0.6858 0.4154 0.6024 0.303 Uiso 1 1 calc R
H25B H 0.6690 0.4628 0.5827 0.303 Uiso 1 1 calc R
H25C H 0.6773 0.4188 0.5494 0.303 Uiso 1 1 calc R
C26 C 0.4347(5) 0.2469(4) 0.5901(3) 0.156(4) Uani 1 1 d .
H26A H 0.4308 0.2186 0.6136 0.235 Uiso 1 1 calc R
H26B H 0.4229 0.2262 0.5611 0.235 Uiso 1 1 calc R
H26C H 0.4087 0.2634 0.5972 0.235 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'
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'
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
O1 Mo1 O1 87.5(3) . 10_556
O1 Mo1 O3 176.0(2) . 12_566
O1 Mo1 O3 92.18(19) 10_556 12_566
O1 Mo1 O3 92.18(19) . 3_565
O1 Mo1 O3 176.0(2) 10_556 3_565
O3 Mo1 O3 87.9(3) 12_566 3_565
O1 Mo1 Mo2 91.62(14) . .
O1 Mo1 Mo2 91.62(14) 10_556 .
O3 Mo1 Mo2 92.35(19) 12_566 .
O3 Mo1 Mo2 92.35(19) 3_565 .
O1 Mo1 O7 88.7(2) . .
O1 Mo1 O7 88.7(2) 10_556 .
O3 Mo1 O7 87.3(2) 12_566 .
O3 Mo1 O7 87.3(2) 3_565 .
Mo2 Mo1 O7 179.6(2) . .
O2 Mo2 O2 87.0(3) . 10_556
O2 Mo2 O4 175.9(2) . 12_566
O2 Mo2 O4 92.53(19) 10_556 12_566
O2 Mo2 O4 92.53(19) . 3_565
O2 Mo2 O4 175.9(2) 10_556 3_565
O4 Mo2 O4 87.6(3) 12_566 3_565
O2 Mo2 Mo1 92.28(14) . .
O2 Mo2 Mo1 92.28(14) 10_556 .
O4 Mo2 Mo1 91.82(19) 12_566 .
O4 Mo2 Mo1 91.82(19) 3_565 .
O2 Mo2 O8 92.3(2) . .
O2 Mo2 O8 92.3(2) 10_556 .
O4 Mo2 O8 83.6(2) 12_566 .
O4 Mo2 O8 83.6(2) 3_565 .
Mo1 Mo2 O8 173.7(2) . .
C1 O1 Mo1 114.9(3) . .
C1 O2 Mo2 116.7(4) . .
C24 O3 Mo1 113.0(6) . 2_665
C24 O4 Mo2 115.5(7) . 2_665
C13 O5 C25 116.6(8) . .
C12 O6 C26 114.9(8) . .
O1 C1 O2 124.3(4) . .
O1 C1 C2 117.7(4) . .
O2 C1 C2 117.7(3) . .
C3 C2 C7 120.0 . .
C3 C2 C1 120.0(4) . .
C7 C2 C1 120.0(4) . .
C4 C3 C2 120.0 . .
C4 C3 H3A 120.0 . .
C2 C3 H3A 120.0 . .
C3 C4 C5 120.0 . .
C3 C4 H4A 120.0 . .
C5 C4 H4A 120.0 . .
C6 C5 C4 120.0 . .
C6 C5 C8 114.2(6) . .
C4 C5 C8 125.8(6) . .
C5 C6 C7 120.0 . .
C5 C6 H6A 120.0 . .
C7 C6 H6A 120.0 . .
C6 C7 C2 120.0 . .
C6 C7 H7A 120.0 . .
C2 C7 H7A 120.0 . .
C9 C8 C5 176.7(6) . .
C8 C9 C10 177.8(12) . .
C11 C10 C15 120.0 . .
C11 C10 C9 117.7(7) . .
C15 C10 C9 122.3(7) . .
C10 C11 C12 120.0 . .
C10 C11 H11A 120.0 . .
C12 C11 H11A 120.0 . .
O6 C12 C13 115.9(7) . .
O6 C12 C11 124.0(7) . .
C13 C12 C11 120.0 . .
O5 C13 C12 113.8(7) . .
O5 C13 C14 126.2(7) . .
C12 C13 C14 120.0 . .
C13 C14 C15 120.0 . .
C13 C14 H14A 120.0 . .
C15 C14 H14A 120.0 . .
C14 C15 C10 120.0 . .
C14 C15 C16 117.0(7) . .
C10 C15 C16 123.0(7) . .
C17 C16 C15 175.2(10) . .
C16 C17 C18 179.1(8) . .
C19 C18 C23 120.0 . .
C19 C18 C17 126.6(10) . .
C23 C18 C17 113.4(10) . .
C18 C19 C20 120.0 . .
C18 C19 H19A 120.0 . .
C20 C19 H19A 120.0 . .
C19 C20 C21 120.0 . .
C19 C20 H20A 120.0 . .
C21 C20 H20A 120.0 . .
C22 C21 C20 120.0 . .
C22 C21 C24 118.6(10) . .
C20 C21 C24 121.4(10) . .
C21 C22 C23 120.0 . .
C21 C22 H22A 120.0 . .
C23 C22 H22A 120.0 . .
C22 C23 C18 120.0 . .
C22 C23 H23A 120.0 . .
C18 C23 H23A 120.0 . .
O4 C24 O3 127.3(10) . .
O4 C24 C21 117.1(10) . .
O3 C24 C21 115.6(10) . .
O5 C25 H25A 109.5 . .
O5 C25 H25B 109.5 . .
H25A C25 H25B 109.5 . .
O5 C25 H25C 109.5 . .
H25A C25 H25C 109.5 . .
H25B C25 H25C 109.5 . .
O6 C26 H26A 109.5 . .
O6 C26 H26B 109.5 . .
H26A C26 H26B 109.5 . .
O6 C26 H26C 109.5 . .
H26A C26 H26C 109.5 . .
H26B C26 H26C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 O1 2.097(5) .
Mo1 O1 2.097(5) 10_556
Mo1 O3 2.098(7) 12_566
Mo1 O3 2.098(7) 3_565
Mo1 Mo2 2.1052(17) .
Mo1 O7 2.4011(10) .
Mo2 O2 2.049(5) .
Mo2 O2 2.049(5) 10_556
Mo2 O4 2.079(6) 12_566
Mo2 O4 2.079(6) 3_565
Mo2 O8 2.4027(10) .
O1 C1 1.270(7) .
O2 C1 1.272(6) .
O3 C24 1.284(10) .
O3 Mo1 2.099(7) 2_665
O4 C24 1.235(9) .
O4 Mo2 2.079(6) 2_665
O5 C13 1.355(7) .
O5 C25 1.391(9) .
O6 C12 1.373(7) .
O6 C26 1.435(9) .
C1 C2 1.504(6) .
C2 C3 1.3900 .
C2 C7 1.3900 .
C3 C4 1.3900 .
C3 H3A 0.9500 .
C4 C5 1.3900 .
C4 H4A 0.9500 .
C5 C6 1.3900 .
C5 C8 1.490(10) .
C6 C7 1.3900 .
C6 H6A 0.9500 .
C7 H7A 0.9500 .
C8 C9 1.153(10) .
C9 C10 1.415(9) .
C10 C11 1.3900 .
C10 C15 1.3900 .
C11 C12 1.3900 .
C11 H11A 0.9500 .
C12 C13 1.3900 .
C13 C14 1.3900 .
C14 C15 1.3900 .
C14 H14A 0.9500 .
C15 C16 1.425(10) .
C16 C17 1.216(10) .
C17 C18 1.402(11) .
C18 C19 1.3900 .
C18 C23 1.3900 .
C19 C20 1.3900 .
C19 H19A 0.9500 .
C20 C21 1.3900 .
C20 H20A 0.9500 .
C21 C22 1.3900 .
C21 C24 1.513(10) .
C22 C23 1.3900 .
C22 H22A 0.9500 .
C23 H23A 0.9500 .
C25 H25A 0.9800 .
C25 H25B 0.9800 .
C25 H25C 0.9800 .
C26 H26A 0.9800 .
C26 H26B 0.9800 .
C26 H26C 0.9800 .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.010 -0.006 -0.002 11488 3140 ' '
