#------------------------------------------------------------------------------
#$Date: 2016-03-21 01:21:50 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178377 $
#$URL: svn://www.crystallography.net/cod/cif/4/00/03/4000369.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_4000369
_journal_name_full               'Chemistry of Materials'
_journal_paper_doi               10.1021/cm030563k
_journal_year                    2004
_chemical_formula_moiety         'C40 H90 Mo2 O12 Si2'
_chemical_formula_sum            'C40 H90 Mo2 O12 Si2'
_chemical_formula_weight         1011.18
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 102.30
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.7732(5)
_cell_length_b                   12.4173(5)
_cell_length_c                   17.3864(7)
_cell_measurement_reflns_used    4842
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.7
_cell_measurement_theta_min      1.75
_cell_volume                     2694.3(2)
_diffrn_ambient_temperature      154(2)
_diffrn_measurement_device       'Bruker SMART CCD'
_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  0.0470
_diffrn_reflns_av_sigmaI/netI    0.0525
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11663
_diffrn_reflns_theta_max         24.69
_diffrn_reflns_theta_min         1.81
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_exptl_absorpt_coefficient_mu    0.559
_exptl_absorpt_correction_T_max  0.94427
_exptl_absorpt_correction_T_min  0.54422
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1076
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.931
_refine_ls_goodness_of_fit_obs   1.060
_refine_ls_hydrogen_treatment    fixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         4418
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.931
_refine_ls_restrained_S_obs      1.060
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_obs          0.0333
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0473P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0828
_refine_ls_wR_factor_obs         0.0785
_reflns_number_observed          3143
_reflns_number_total             4418
_reflns_observed_criterion       >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0473P)^2^+0.0000P] 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^)+(0.0473P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4000369
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Mo1 Mo 0.43195(2) 0.49566(3) 0.03152(4) 0.0177(2) Uani 0.916(2) d P .
Mo2 Mo 0.4164(3) 0.4705(3) -0.0188(6) 0.035(2) Uani 0.084(2) d P .
Si1 Si 0.33083(6) 0.27105(6) 0.07520(5) 0.0240(2) Uani 1 d . .
O1 O 0.3982(2) 0.3439(2) 0.02519(12) 0.0279(5) Uani 1 d . .
O2 O 0.3965(2) 0.16284(15) 0.10764(12) 0.0291(5) Uani 1 d . .
O3 O 0.21484(15) 0.2332(2) 0.02540(12) 0.0296(5) Uani 1 d . .
O4 O 0.3077(2) 0.35022(15) 0.14399(12) 0.0275(5) Uani 1 d . .
O5 O 0.4810(2) 0.5502(2) 0.13259(12) 0.0319(5) Uani 1 d . .
O6 O 0.3367(2) 0.5896(2) -0.03447(12) 0.0306(5) Uani 1 d . .
C1 C 0.5088(3) 0.1454(2) 0.1414(2) 0.0397(9) Uani 1 d . .
C2 C 0.5555(3) 0.2402(3) 0.1926(2) 0.0516(11) Uani 1 d . .
H2A H 0.5187(3) 0.2482(3) 0.2349(2) 0.077 Uiso 1 calc R .
H2B H 0.5472(3) 0.3047(3) 0.1614(2) 0.077 Uiso 1 calc R .
H2C H 0.6303(3) 0.2276(3) 0.2137(2) 0.077 Uiso 1 calc R .
C3 C 0.5663(3) 0.1318(3) 0.0741(3) 0.0590(12) Uani 1 d . .
H3A H 0.5362(3) 0.0717(3) 0.0422(3) 0.089 Uiso 1 calc R .
H3B H 0.6411(3) 0.1189(3) 0.0950(3) 0.089 Uiso 1 calc R .
H3C H 0.5580(3) 0.1960(3) 0.0427(3) 0.089 Uiso 1 calc R .
C4 C 0.5130(3) 0.0423(3) 0.1892(3) 0.077(2) Uani 1 d . .
H4A H 0.4762(3) 0.0531(3) 0.2313(3) 0.115 Uiso 1 calc R .
H4B H 0.5863(3) 0.0237(3) 0.2107(3) 0.115 Uiso 1 calc R .
H4C H 0.4791(3) -0.0148(3) 0.1558(3) 0.115 Uiso 1 calc R .
C5 C 0.1774(3) 0.1457(3) -0.0283(2) 0.0342(8) Uani 1 d . .
C6 C 0.2480(3) 0.1359(3) -0.0880(2) 0.0535(11) Uani 1 d . .
H6A H 0.2464(3) 0.2023(3) -0.1165(2) 0.080 Uiso 1 calc R .
H6B H 0.2222(3) 0.0785(3) -0.1240(2) 0.080 Uiso 1 calc R .
H6C H 0.3203(3) 0.1207(3) -0.0611(2) 0.080 Uiso 1 calc R .
C7 C 0.1771(4) 0.0430(3) 0.0183(2) 0.0649(13) Uani 1 d . .
H7A H 0.2493(4) 0.0246(3) 0.0435(2) 0.097 Uiso 1 calc R .
H7B H 0.1465(4) -0.0142(3) -0.0164(2) 0.097 Uiso 1 calc R .
H7C H 0.1354(4) 0.0533(3) 0.0576(2) 0.097 Uiso 1 calc R .
C8 C 0.0646(3) 0.1774(3) -0.0689(2) 0.0592(12) Uani 1 d . .
H8A H 0.0668(3) 0.2427(3) -0.0981(2) 0.089 Uiso 1 calc R .
H8B H 0.0222(3) 0.1886(3) -0.0302(2) 0.089 Uiso 1 calc R .
H8C H 0.0333(3) 0.1210(3) -0.1042(2) 0.089 Uiso 1 calc R .
C9 C 0.2405(2) 0.3359(3) 0.2006(2) 0.0321(8) Uani 1 d . .
C10 C 0.2464(3) 0.2207(3) 0.2301(2) 0.0537(11) Uani 1 d . .
H10A H 0.2193(3) 0.1730(3) 0.1870(2) 0.081 Uiso 1 calc R .
H10B H 0.2042(3) 0.2135(3) 0.2694(2) 0.081 Uiso 1 calc R .
H10C H 0.3196(3) 0.2026(3) 0.2527(2) 0.081 Uiso 1 calc R .
C11 C 0.1260(3) 0.3647(3) 0.1612(2) 0.0484(10) Uani 1 d . .
H11A H 0.1003(3) 0.3152(3) 0.1190(2) 0.073 Uiso 1 calc R .
H11B H 0.1240(3) 0.4366(3) 0.1407(2) 0.073 Uiso 1 calc R .
H11C H 0.0814(3) 0.3605(3) 0.1991(2) 0.073 Uiso 1 calc R .
C12 C 0.2827(3) 0.4128(3) 0.2672(2) 0.0558(11) Uani 1 d . .
H12A H 0.2783(3) 0.4852(3) 0.2474(2) 0.084 Uiso 1 calc R .
H12B H 0.3560(3) 0.3955(3) 0.2899(2) 0.084 Uiso 1 calc R .
H12C H 0.2406(3) 0.4064(3) 0.3066(2) 0.084 Uiso 1 calc R .
C13 C 0.5602(2) 0.6097(2) 0.1877(2) 0.0282(7) Uani 1 d . .
C14 C 0.5422(3) 0.5786(3) 0.2685(2) 0.0497(10) Uani 1 d . .
H14A H 0.4713(3) 0.5996(3) 0.2728(2) 0.074 Uiso 1 calc R .
H14B H 0.5940(3) 0.6145(3) 0.3084(2) 0.074 Uiso 1 calc R .
H14C H 0.5500(3) 0.5021(3) 0.2754(2) 0.074 Uiso 1 calc R .
C15 C 0.5388(3) 0.7284(2) 0.1707(2) 0.0420(9) Uani 1 d . .
H15A H 0.4676(3) 0.7458(2) 0.1765(2) 0.063 Uiso 1 calc R .
H15B H 0.5454(3) 0.7440(2) 0.1179(2) 0.063 Uiso 1 calc R .
H15C H 0.5897(3) 0.7706(2) 0.2070(2) 0.063 Uiso 1 calc R .
C16 C 0.6716(3) 0.5773(3) 0.1795(2) 0.0495(10) Uani 1 d . .
H16A H 0.6821(3) 0.5019(3) 0.1907(2) 0.074 Uiso 1 calc R .
H16B H 0.7238(3) 0.6181(3) 0.2159(2) 0.074 Uiso 1 calc R .
H16C H 0.6795(3) 0.5915(3) 0.1268(2) 0.074 Uiso 1 calc R .
C17 C 0.2276(2) 0.6158(3) -0.0269(2) 0.0381(9) Uani 1 d . .
C18 C 0.1607(3) 0.5150(3) -0.0334(3) 0.075(2) Uani 1 d . .
H18A H 0.1894(3) 0.4678(3) 0.0096(3) 0.113 Uiso 1 calc R .
H18B H 0.1618(3) 0.4795(3) -0.0823(3) 0.113 Uiso 1 calc R .
H18C H 0.0882(3) 0.5336(3) -0.0317(3) 0.113 Uiso 1 calc R .
C19 C 0.1836(3) 0.6900(3) -0.0936(3) 0.078(2) Uani 1 d . .
H19A H 0.2266(3) 0.7540(3) -0.0891(3) 0.117 Uiso 1 calc R .
H19B H 0.1112(3) 0.7088(3) -0.0921(3) 0.117 Uiso 1 calc R .
H19C H 0.1847(3) 0.6547(3) -0.1426(3) 0.117 Uiso 1 calc R .
C20 C 0.2353(4) 0.6699(6) 0.0517(3) 0.137(3) Uani 1 d . .
H20A H 0.2638(4) 0.6200(6) 0.0930(3) 0.205 Uiso 1 calc R .
H20B H 0.1653(4) 0.6928(6) 0.0568(3) 0.205 Uiso 1 calc R .
H20C H 0.2817(4) 0.7313(6) 0.0552(3) 0.205 Uiso 1 calc R .
