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#$Date: 2016-03-23 21:40:04 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179454 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/51/4335157.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_4335157
loop_
_publ_author_name
'Maria V. Ivanova'
'Tobias Köchner'
'Hélène P. A. Mercier'
'Gary J. Schrobilgen'
_publ_section_title
;
 Synthesis and Lewis Acid Properties of (ReO3F)∞ and the X-ray
 Crystal Structures of (HF)2ReO3F.HF and
 [N(CH3)4]2-[{ReO3(μ-F)}3(μ3-O)].CH3CN
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6806
_journal_page_last               6819
_journal_paper_doi               10.1021/ic302221y
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C4 H12 N, O4 Re'
_chemical_formula_sum            'C4 H12 N O4 Re'
_chemical_formula_weight         324.35
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 115.7730(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.7206(2)
_cell_length_b                   12.4740(3)
_cell_length_c                   13.1586(4)
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      78
_cell_measurement_theta_min      0
_cell_volume                     845.58(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_molecular_graphics    'SHELXTL V6.10 2001  Bruker-AXS'
_computing_publication_material  'SHELXTL V6.10 2001  Bruker-AXS'
_computing_structure_refinement  'SHELXTL V6.10 2001  Bruker-AXS'
_computing_structure_solution    'SHELXTL V6.10 2001  Bruker-AXS'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  '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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0473
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4944
_diffrn_reflns_theta_full        39.01
_diffrn_reflns_theta_max         39.01
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    14.335
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.469
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2.10'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.548
_exptl_crystal_description       block
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.884
_refine_diff_density_min         -4.242
_refine_diff_density_rms         0.329
_refine_ls_extinction_coef       0.0092(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.909
_refine_ls_matrix_type           full
_refine_ls_number_parameters     102
_refine_ls_number_reflns         4944
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.909
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0343
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0635P)²+4.5547P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0947
_refine_ls_wR_factor_ref         0.1032
_reflns_number_gt                4090
_reflns_number_total             4944
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302221y_si_002_2.cif
_cod_data_source_block           N(CH3)4ReO4
_cod_original_cell_volume        845.57(4)
_cod_database_code               4335157
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, 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
_atom_site_refinement_flags
Re1 Re 0.96339(4) 0.7500 0.016695(18) 0.01032(6) Uani 1 2 d S
Re2 Re 0.42994(4) 0.2500 0.483201(18) 0.01024(6) Uani 1 2 d S
N1 N 0.7739(7) 0.5003(3) 0.2502(3) 0.0106(5) Uani 1 1 d .
C1 C 0.6842(10) 0.4210(4) 0.3109(4) 0.0168(8) Uani 1 1 d .
H1A H 0.6428 0.4578 0.3651 0.025 Uiso 1 1 calc R
H1B H 0.8195 0.3698 0.3491 0.025 Uiso 1 1 calc R
H1C H 0.5327 0.3845 0.2576 0.025 Uiso 1 1 calc R
C2 C 0.5631(9) 0.5796(4) 0.1894(4) 0.0166(7) Uani 1 1 d .
H2A H 0.5202 0.6169 0.2429 0.025 Uiso 1 1 calc R
H2B H 0.4123 0.5427 0.1361 0.025 Uiso 1 1 calc R
H2C H 0.6213 0.6300 0.1503 0.025 Uiso 1 1 calc R
C3 C 0.8396(10) 0.4427(4) 0.1660(4) 0.0181(8) Uani 1 1 d .
H3A H 0.9748 0.3915 0.2044 0.027 Uiso 1 1 calc R
H3B H 0.8977 0.4935 0.1271 0.027 Uiso 1 1 calc R
H3C H 0.6884 0.4062 0.1125 0.027 Uiso 1 1 calc R
C4 C 1.0070(10) 0.5578(5) 0.3335(4) 0.0194(8) Uani 1 1 d .
H4A H 0.9632 0.5943 0.3872 0.029 Uiso 1 1 calc R
H4B H 1.0646 0.6090 0.2949 0.029 Uiso 1 1 calc R
H4C H 1.1432 0.5071 0.3723 0.029 Uiso 1 1 calc R
O1 O 1.2497(10) 0.7500 0.0021(4) 0.0150(8) Uani 1 2 d S
O6 O 0.7440(10) 0.2500 0.4949(5) 0.0175(9) Uani 1 2 d S
O4 O 0.2131(12) 0.2500 0.3415(4) 0.0231(11) Uani 1 2 d S
O5 O 0.3824(9) 0.3634(4) 0.5465(4) 0.0264(9) Uani 1 1 d .
O2 O 0.7888(9) 0.6357(4) -0.0456(4) 0.0262(8) Uani 1 1 d .
O3 O 1.0329(12) 0.7500 0.1581(4) 0.0230(11) Uani 1 2 d S
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
Re1 0.01252(11) 0.01023(10) 0.00835(10) 0.000 0.00466(8) 0.000
Re2 0.01230(11) 0.01018(10) 0.00815(10) 0.000 0.00436(7) 0.000
N1 0.0137(15) 0.0105(13) 0.0082(11) 0.0006(10) 0.0054(11) 0.0010(12)
C1 0.020(2) 0.0169(18) 0.0169(18) 0.0020(15) 0.0112(16) -0.0014(15)
C2 0.0147(18) 0.0142(17) 0.0180(18) 0.0044(14) 0.0045(15) 0.0020(14)
C3 0.021(2) 0.022(2) 0.0140(17) -0.0023(15) 0.0103(16) 0.0026(17)
C4 0.0145(18) 0.027(2) 0.0121(16) -0.0020(16) 0.0015(14) -0.0048(17)
O1 0.016(2) 0.017(2) 0.016(2) 0.000 0.0109(17) 0.000
O6 0.013(2) 0.015(2) 0.023(2) 0.000 0.0057(18) 0.000
O4 0.021(3) 0.030(3) 0.0062(17) 0.000 -0.0048(17) 0.000
O5 0.026(2) 0.0235(19) 0.033(2) -0.0126(16) 0.0162(18) -0.0022(16)
O2 0.0236(19) 0.0236(19) 0.033(2) -0.0120(16) 0.0138(17) -0.0105(16)
O3 0.030(3) 0.032(3) 0.0094(18) 0.000 0.010(2) 0.000
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'
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
O3 Re1 O1 109.5(3) . .
O3 Re1 O2 109.03(19) . .
O1 Re1 O2 109.06(16) . .
O3 Re1 O2 109.03(19) . 4_575
O1 Re1 O2 109.06(16) . 4_575
O2 Re1 O2 111.1(3) . 4_575
O5 Re2 O5 110.4(3) 4_565 .
O5 Re2 O4 109.3(2) 4_565 .
O5 Re2 O4 109.3(2) . .
O5 Re2 O6 109.41(17) 4_565 .
O5 Re2 O6 109.41(17) . .
O4 Re2 O6 108.9(3) . .
C1 N1 C4 109.3(4) . .
C1 N1 C3 109.4(4) . .
C4 N1 C3 110.1(3) . .
C1 N1 C2 109.8(3) . .
C4 N1 C2 109.3(4) . .
C3 N1 C2 109.0(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Re1 O3 1.725(5) .
Re1 O1 1.730(5) .
Re1 O2 1.730(4) .
Re1 O2 1.730(4) 4_575
Re2 O5 1.722(4) 4_565
Re2 O5 1.722(4) .
Re2 O4 1.733(5) .
Re2 O6 1.735(5) .
N1 C1 1.496(6) .
N1 C4 1.492(6) .
N1 C3 1.499(5) .
N1 C2 1.495(6) .
