#------------------------------------------------------------------------------
#$Date: 2013-12-29 13:49:26 +0200 (Sun, 29 Dec 2013) $
#$Revision: 91935 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/00/16/4001640.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_4001640
loop_
_publ_author_name
'Shcheglov, Pavel A.'
'Drobot, Dmitry V.'
'Seisenbaeva, Gulaim A.'
'Gohil, Suresh'
'Kessler, Vadim G.'
_publ_section_title
;
 Alkoxide Route to Mixed Oxides of Rhenium, Niobium, and Tantalum.
 Preparation and X-ray Single-Crystal Study of a Novel
 Rhenium−Niobium Methoxo Complex, Nb2(OMe)8(ReO4)2
;
_journal_issue                   5
_journal_name_full               'Chemistry of Materials'
_journal_page_first              2378
_journal_volume                  14
_journal_year                    2002
_chemical_formula_sum            'C8 H24 Nb2 O16 Re2'
_chemical_formula_weight         934.49
_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                90.00
_cell_angle_beta                 97.31(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.5609(16)
_cell_length_b                   12.890(3)
_cell_length_c                   10.652(3)
_cell_measurement_reflns_used    7517(I>2sigma(I))
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      22.50
_cell_measurement_theta_min      2.40
_cell_volume                     1165.9(5)
_computing_cell_refinement       'Bruker SAINTPLUS'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINTPLUS'
_computing_molecular_graphics    'Bruker SHELXTL-NT'
_computing_publication_material  'Bruker SHELXTL-NT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker SMART CCD 1K'
_diffrn_measurement_method       'Bruker SMART'
_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  0.1362
_diffrn_reflns_av_sigmaI/netI    0.1410
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4693
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.40
_exptl_absorpt_coefficient_mu    11.371
_exptl_absorpt_correction_T_max  0.4632
_exptl_absorpt_correction_T_min  0.2803
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    2.662
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.103
_refine_diff_density_min         -1.724
_refine_diff_density_rms         0.235
_refine_ls_extinction_coef       0.0015(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.902
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     117
_refine_ls_number_reflns         1514
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.902
_refine_ls_R_factor_all          0.1419
_refine_ls_R_factor_gt           0.0679
_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/[\s^2^(Fo^2^)+(0.0798P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1417
_refine_ls_wR_factor_ref         0.1604
_reflns_number_gt                804
_reflns_number_total             1514
_reflns_threshold_expression     >2sigma(I)
_[local]_cod_data_source_file    cm011726c.cif
_[local]_cod_data_source_block   renb2m
_[local]_cod_cif_authors_sg_H-M  P2(1)/c
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               4001640
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
Re Re 0.11977(13) 0.01330(12) 0.21032(11) 0.0824(7) Uani 1 1 d .
Nb Nb 0.4906(2) 0.10446(17) 0.4000(2) 0.0418(7) Uani 1 1 d .
O3 O 0.5314(19) 0.1078(12) 0.2374(14) 0.062(5) Uani 1 1 d .
O1 O 0.4498(15) 0.0500(10) 0.5829(13) 0.039(4) Uani 1 1 d .
O8 O -0.026(3) -0.049(2) 0.257(2) 0.129(8) Uiso 1 1 d .
O4 O 0.6811(15) 0.1551(13) 0.4641(16) 0.064(5) Uani 1 1 d .
O2 O 0.3769(16) 0.2209(13) 0.4184(13) 0.056(4) Uani 1 1 d .
O7 O 0.033(3) 0.134(2) 0.155(3) 0.150(10) Uiso 1 1 d .
O5 O 0.2652(17) 0.0362(12) 0.3339(15) 0.063(5) Uani 1 1 d .
C1 C 0.432(3) 0.1235(18) 0.682(2) 0.076(9) Uani 1 1 d .
H1A H 0.3370 0.1088 0.7174 0.114 Uiso 1 1 calc R
H1B H 0.4271 0.1924 0.6473 0.114 Uiso 1 1 calc R
H1C H 0.5206 0.1182 0.7466 0.114 Uiso 1 1 calc R
O6 O 0.185(4) -0.043(3) 0.102(4) 0.216(15) Uiso 1 1 d .
C2 C 0.228(3) 0.268(2) 0.421(3) 0.083(9) Uani 1 1 d .
H2A H 0.1673 0.2615 0.3389 0.125 Uiso 1 1 calc R
H2B H 0.2420 0.3399 0.4419 0.125 Uiso 1 1 calc R
H2C H 0.1739 0.2340 0.4829 0.125 Uiso 1 1 calc R
C4 C 0.839(2) 0.176(2) 0.469(3) 0.088(10) Uani 1 1 d .
H4A H 0.8969 0.1123 0.4696 0.132 Uiso 1 1 calc R
H4B H 0.8740 0.2144 0.5452 0.132 Uiso 1 1 calc R
H4C H 0.8573 0.2167 0.3969 0.132 Uiso 1 1 calc R
C3 C 0.618(3) 0.105(2) 0.135(2) 0.086(9) Uani 1 1 d .
H3A H 0.6487 0.1746 0.1153 0.129 Uiso 1 1 calc R
H3B H 0.5548 0.0761 0.0625 0.129 Uiso 1 1 calc R
H3C H 0.7106 0.0635 0.1559 0.129 Uiso 1 1 calc R
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
Re 0.0558(7) 0.1310(15) 0.0577(8) -0.0138(8) -0.0031(5) -0.0156(8)
Nb 0.0369(11) 0.0418(14) 0.0485(13) 0.0017(11) 0.0124(9) -0.0026(11)
O3 0.088(11) 0.044(11) 0.055(10) 0.014(8) 0.018(9) 0.021(9)
O1 0.052(8) 0.006(8) 0.062(10) -0.011(7) 0.023(8) -0.010(7)
O4 0.037(9) 0.056(11) 0.100(13) -0.014(10) 0.014(8) -0.027(8)
O2 0.051(9) 0.072(13) 0.048(10) 0.007(9) 0.015(8) -0.012(9)
O5 0.054(9) 0.077(14) 0.063(10) 0.002(9) 0.021(8) 0.005(9)
C1 0.14(2) 0.041(18) 0.051(16) -0.025(14) 0.023(16) -0.008(17)
C2 0.08(2) 0.07(2) 0.11(3) -0.006(18) 0.032(18) 0.009(17)
C4 0.042(14) 0.12(3) 0.10(2) -0.01(2) -0.005(14) -0.025(17)
C3 0.10(2) 0.10(3) 0.060(19) 0.004(18) 0.039(17) 0.015(19)
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'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.0185 7.2310 '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
O6 Re O8 111.3(17) . .
O6 Re O5 111.4(15) . .
O8 Re O5 111.2(10) . .
O6 Re O7 109.8(16) . .
O8 Re O7 103.3(12) . .
O5 Re O7 109.5(10) . .
O4 Nb O3 94.5(8) . .
O4 Nb O2 97.6(7) . .
O3 Nb O2 104.8(6) . .
O4 Nb O1 96.6(7) . 3_656
O3 Nb O1 91.9(6) . 3_656
O2 Nb O1 157.2(6) . 3_656
O4 Nb O1 91.1(6) . .
O3 Nb O1 162.2(6) . .
O2 Nb O1 91.2(6) . .
O1 Nb O1 70.7(6) 3_656 .
O4 Nb O5 176.1(7) . .
O3 Nb O5 88.3(7) . .
O2 Nb O5 84.4(6) . .
O1 Nb O5 80.5(6) 3_656 .
O1 Nb O5 85.4(5) . .
C3 O3 Nb 159.0(16) . .
C1 O1 Nb 128.3(14) . 3_656
C1 O1 Nb 119.7(13) . .
Nb O1 Nb 109.3(6) 3_656 .
C4 O4 Nb 157.4(17) . .
C2 O2 Nb 148.6(15) . .
Re O5 Nb 148.4(9) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Re O6 1.53(4) .
Re O8 1.62(3) .
Re O5 1.718(16) .
Re O7 1.79(3) .
Nb O4 1.808(13) .
Nb O3 1.811(15) .
Nb O2 1.813(16) .
Nb O1 2.057(13) 3_656
Nb O1 2.140(14) .
Nb O5 2.156(15) .
O3 C3 1.40(3) .
O1 C1 1.44(2) .
O1 Nb 2.057(13) 3_656
O4 C4 1.38(2) .
O2 C2 1.41(3) .
_journal_paper_doi 10.1021/cm011726c