#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:01:48 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179436 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/33/4333397.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_4333397
loop_
_publ_author_name
'Li, Bo'
'Zhang, Haitao'
'Huynh, Lan'
'Shatruk, Mikhael'
'Dikarev, Evgeny V.'
_publ_section_title
;
 Mo/Rh Carboxylate:  Heterometallic Compound Built of Homometallic
 Paddlewheel Units
;
_journal_issue                   22
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9155
_journal_page_last               9159
_journal_paper_doi               10.1021/ic7009012
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'Mo2 (O2 C C F3)4'
_chemical_formula_sum            'C8 F12 Mo2 O8'
_chemical_formula_weight         643.96
_chemical_melting_point          ?
_chemical_name_systematic
; 
 tetrakis(mu2-trifluoroacetateo-O,O')-di-molybdenium(II)  
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                87.515(2)
_cell_angle_beta                 85.862(2)
_cell_angle_gamma                80.617(2)
_cell_formula_units_Z            1
_cell_length_a                   5.5662(8)
_cell_length_b                   8.2207(12)
_cell_length_c                   8.9579(13)
_cell_measurement_reflns_used    3332
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.03
_cell_measurement_theta_min      2.28
_cell_volume                     403.15(10)
_computing_cell_refinement       'SMART, SAINT'
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXP-93 (Sheldrick, 1993)'
_computing_publication_material  'SHELXCIF-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.904
_diffrn_measured_fraction_theta_max 0.904
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       '0.3 deg wide ω exposures'
_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  0.0175
_diffrn_reflns_av_sigmaI/netI    0.0248
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3445
_diffrn_reflns_theta_full        28.03
_diffrn_reflns_theta_max         28.03
_diffrn_reflns_theta_min         2.28
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count na
_diffrn_standards_interval_time  na
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    1.729
_exptl_absorpt_correction_T_max  0.8741
_exptl_absorpt_correction_T_min  0.3995
_exptl_absorpt_correction_type   'multi-scan (SADABS)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.652
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       needle
_exptl_crystal_F_000             304
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.551
_refine_diff_density_min         -0.731
_refine_diff_density_rms         0.098
_refine_ls_extinction_coef       0.040(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         1768
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0222
_refine_ls_R_factor_gt           0.0220
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0341P)²+0.3390P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0574
_refine_ls_wR_factor_ref         0.0576
_reflns_number_gt                1738
_reflns_number_total             1768
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic7009012sup1.cif
_cod_data_source_block           '[Mo2(O2CCF3)4]'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

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_database_code               4333397
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Mo1 Mo 0.35331(3) 0.439325(18) 0.037349(17) 0.01815(10) Uani 1 1 d
O1 O 0.3711(3) 0.31870(19) -0.16641(18) 0.0235(3) Uani 1 1 d
O2 O 0.3160(3) 0.55352(19) 0.24538(18) 0.0234(3) Uani 1 1 d
O3 O 0.5863(3) 0.23859(19) 0.13260(17) 0.0208(3) Uani 1 1 d
O4 O 0.0992(3) 0.63449(19) -0.05578(18) 0.0209(3) Uani 1 1 d
C1 C 0.4684(4) 0.6471(3) 0.2635(2) 0.0242(4) Uani 1 1 d
C2 C 0.4613(5) 0.7295(3) 0.4148(3) 0.0334(5) Uani 1 1 d
C3 C 0.1918(4) 0.7516(2) -0.1222(2) 0.0204(4) Uani 1 1 d
C4 C 0.0124(4) 0.8867(3) -0.1979(3) 0.0250(4) Uani 1 1 d
F1 F 0.3726(5) 0.8880(2) 0.4012(2) 0.0648(6) Uani 1 1 d
F2 F 0.3263(4) 0.6601(2) 0.51972(18) 0.0501(4) Uani 1 1 d
F3 F 0.6825(4) 0.7159(3) 0.4626(2) 0.0524(5) Uani 1 1 d
F4 F 0.1216(3) 1.0045(2) -0.2604(3) 0.0551(5) Uani 1 1 d
F5 F -0.1620(3) 0.9528(2) -0.09909(18) 0.0400(4) Uani 1 1 d
F6 F -0.0971(3) 0.8196(2) -0.30039(18) 0.0395(4) Uani 1 1 d
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mo1 0.01227(13) 0.02114(13) 0.02243(13) -0.00017(7) -0.00291(7) -0.00622(7)
O1 0.0225(8) 0.0243(7) 0.0256(8) -0.0025(6) -0.0059(6) -0.0068(6)
O2 0.0209(8) 0.0268(8) 0.0226(7) -0.0014(6) -0.0007(6) -0.0044(6)
O3 0.0148(7) 0.0228(7) 0.0261(8) 0.0009(6) -0.0035(6) -0.0063(6)
O4 0.0126(7) 0.0237(7) 0.0273(8) 0.0022(6) -0.0045(6) -0.0050(6)
C1 0.0250(10) 0.0233(10) 0.0242(10) -0.0030(8) -0.0061(8) -0.0009(8)
C2 0.0432(14) 0.0289(11) 0.0281(11) -0.0043(9) -0.0079(10) -0.0020(10)
C3 0.0190(10) 0.0209(9) 0.0222(9) -0.0014(7) -0.0027(7) -0.0049(7)
C4 0.0202(10) 0.0249(10) 0.0310(11) 0.0005(8) -0.0043(8) -0.0062(8)
F1 0.1109(19) 0.0315(9) 0.0467(10) -0.0134(7) -0.0212(11) 0.0147(10)
F2 0.0648(12) 0.0568(11) 0.0295(8) -0.0118(7) 0.0077(8) -0.0139(9)
F3 0.0541(11) 0.0704(12) 0.0371(9) -0.0123(8) -0.0205(8) -0.0125(9)
F4 0.0324(8) 0.0425(9) 0.0917(15) 0.0363(10) -0.0161(9) -0.0144(7)
F5 0.0306(8) 0.0422(8) 0.0435(9) -0.0106(7) -0.0067(6) 0.0097(6)
F6 0.0401(9) 0.0407(8) 0.0379(8) -0.0065(6) -0.0195(7) 0.0023(7)
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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 Mo1 91.61(5) . 2_665
O1 Mo1 O2 176.43(5) . .
Mo1 Mo1 O2 91.94(5) 2_665 .
O1 Mo1 O3 91.29(6) . .
Mo1 Mo1 O3 92.64(4) 2_665 .
O2 Mo1 O3 88.85(6) . .
O1 Mo1 O4 88.27(6) . .
Mo1 Mo1 O4 90.84(4) 2_665 .
O2 Mo1 O4 91.37(6) . .
O3 Mo1 O4 176.50(5) . .
C1 O1 Mo1 115.72(13) 2_665 .
C1 O2 Mo1 115.34(14) . .
C3 O3 Mo1 115.88(13) 2_665 .
C3 O4 Mo1 115.67(13) . .
O2 C1 O1 125.3(2) . 2_665
O2 C1 C2 118.7(2) . .
O1 C1 C2 115.9(2) 2_665 .
F3 C2 F1 108.0(2) . .
F3 C2 F2 107.1(2) . .
F1 C2 F2 109.0(2) . .
F3 C2 C1 110.7(2) . .
F1 C2 C1 110.16(19) . .
F2 C2 C1 111.7(2) . .
O3 C3 O4 124.93(19) 2_665 .
O3 C3 C4 119.07(18) 2_665 .
O4 C3 C4 115.97(18) . .
F4 C4 F6 109.6(2) . .
F4 C4 F5 108.7(2) . .
F6 C4 F5 106.65(19) . .
F4 C4 C3 112.03(18) . .
F6 C4 C3 109.13(17) . .
F5 C4 C3 110.62(18) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 O1 2.1032(16) .
Mo1 Mo1 2.1036(4) 2_665
Mo1 O2 2.1046(16) .
Mo1 O3 2.1149(15) .
Mo1 O4 2.1412(15) .
O1 C1 1.258(3) 2_665
O2 C1 1.257(3) .
O3 C3 1.247(3) 2_665
O4 C3 1.271(3) .
C1 O1 1.258(3) 2_665
C1 C2 1.537(3) .
C2 F3 1.319(3) .
C2 F1 1.319(3) .
C2 F2 1.328(3) .
C3 O3 1.247(3) 2_665
C3 C4 1.537(3) .
C4 F4 1.310(3) .
C4 F6 1.324(3) .
C4 F5 1.329(3) .
