#------------------------------------------------------------------------------
#$Date: 2019-11-23 10:03:17 +0200 (Sat, 23 Nov 2019) $
#$Revision: 232801 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/81/4348161.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_4348161
loop_
_publ_author_name
'Johnstone, Erik V.'
'Poineau, Frederic'
'Todorova, Tanya K.'
'Forster, Paul M.'
'Sørensen, Lasse K'
'Fdez Galván, Ignacio'
'Lindh, Roland'
'Czerwinski, Kenneth R.'
'Sattelberger, Alfred P.'
_publ_section_title
;
 Molecular and Electronic Structure of Re2Br4(PMe3)4.
;
_journal_issue                   14
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7111
_journal_page_last               7116
_journal_paper_doi               10.1021/acs.inorgchem.6b01052
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C12 H36 Br4 P4 Re2'
_chemical_formula_weight         996.33
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 115.1560(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.0461(13)
_cell_length_b                   9.3406(7)
_cell_length_c                   17.1624(12)
_cell_measurement_reflns_used    9958
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      61.027
_cell_measurement_theta_min      4.985
_cell_volume                     2618.5(3)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0269
_diffrn_reflns_av_unetI/netI     0.0187
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            21134
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.528
_diffrn_reflns_theta_min         2.512
_exptl_absorpt_coefficient_mu    15.581
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.4333
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1272 before and 0.0391 after correction.
The Ratio of minimum to maximum transmission is 0.5808.
The λ/2 correction factor is 0.00150.
;
_exptl_crystal_density_diffrn    2.527
_exptl_crystal_description       block
_exptl_crystal_F_000             1832
_exptl_crystal_size_max          .10
_exptl_crystal_size_mid          .06
_exptl_crystal_size_min          .04
_refine_diff_density_max         0.894
_refine_diff_density_min         -2.555
_refine_diff_density_rms         0.262
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     101
_refine_ls_number_reflns         3994
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0274
_refine_ls_R_factor_gt           0.0261
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0265P)²+43.5099P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0665
_refine_ls_wR_factor_ref         0.0671
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3822
_reflns_number_total             3994
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic6b01052_si_001.cif
_cod_data_source_block           ReBrTMP_0m_a
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4348161
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Re1 Re 0.5000 0.40875(2) 0.2500 0.00924(6) Uani 1 2 d S T P
Re2 Re 0.5000 0.16765(2) 0.2500 0.00980(6) Uani 1 2 d S T P
Br1 Br 0.41748(3) 0.51745(6) 0.32079(3) 0.02480(11) Uani 1 1 d . . .
Br2 Br 0.38742(3) 0.05842(6) 0.12037(3) 0.02616(11) Uani 1 1 d . . .
P1 P 0.61700(7) 0.45871(13) 0.38422(7) 0.0150(2) Uani 1 1 d . . .
P2 P 0.58683(7) 0.11830(13) 0.17769(8) 0.0166(2) Uani 1 1 d . . .
C1 C 0.6279(4) 0.6530(6) 0.3953(4) 0.0309(12) Uani 1 1 d . . .
H1A H 0.5760 0.6952 0.3893 0.046 Uiso 1 1 calc R U .
H1B H 0.6710 0.6767 0.4521 0.046 Uiso 1 1 calc R U .
H1C H 0.6424 0.6913 0.3505 0.046 Uiso 1 1 calc R U .
C2 C 0.6175(3) 0.4085(6) 0.4867(3) 0.0250(10) Uani 1 1 d . . .
H2A H 0.5649 0.4340 0.4868 0.038 Uiso 1 1 calc R U .
H2B H 0.6262 0.3051 0.4952 0.038 Uiso 1 1 calc R U .
H2C H 0.6617 0.4594 0.5333 0.038 Uiso 1 1 calc R U .
C3 C 0.7180(3) 0.4034(6) 0.3972(3) 0.0243(10) Uani 1 1 d . . .
H3A H 0.7245 0.4258 0.3446 0.036 Uiso 1 1 calc R U .
H3B H 0.7598 0.4544 0.4460 0.036 Uiso 1 1 calc R U .
H3C H 0.7243 0.3000 0.4079 0.036 Uiso 1 1 calc R U .
C4 C 0.6942(3) 0.1746(6) 0.2259(4) 0.0287(11) Uani 1 1 d . . .
H4A H 0.7188 0.1517 0.2875 0.043 Uiso 1 1 calc R U .
H4B H 0.7238 0.1241 0.1978 0.043 Uiso 1 1 calc R U .
H4C H 0.6973 0.2780 0.2183 0.043 Uiso 1 1 calc R U .
C5 C 0.5534(4) 0.1694(6) 0.0658(3) 0.0270(11) Uani 1 1 d . . .
H5A H 0.5463 0.2735 0.0603 0.041 Uiso 1 1 calc R U .
H5B H 0.5946 0.1399 0.0460 0.041 Uiso 1 1 calc R U .
H5C H 0.5012 0.1224 0.0307 0.041 Uiso 1 1 calc R U .
C6 C 0.5958(4) -0.0755(6) 0.1727(4) 0.0282(11) Uani 1 1 d . . .
H6A H 0.6139 -0.1160 0.2306 0.042 Uiso 1 1 calc R U .
H6B H 0.5425 -0.1161 0.1348 0.042 Uiso 1 1 calc R U .
H6C H 0.6359 -0.0986 0.1501 0.042 Uiso 1 1 calc R U .
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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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
Re2 Re1 P1 101.13(3) . 2_655
Re2 Re1 P1 101.13(3) . .
P1 Re1 P1 157.75(6) 2_655 .
Re2 Re1 Br1 113.937(13) . 2_655
P1 Re1 Br1 85.30(3) 2_655 2_655
P1 Re1 Br1 85.72(3) . 2_655
Re2 Re1 Br1 113.936(13) . .
P1 Re1 Br1 85.72(3) 2_655 .
P1 Re1 Br1 85.30(3) . .
Br1 Re1 Br1 132.13(3) 2_655 .
Re1 Re2 P2 100.98(3) . .
Re1 Re2 P2 100.98(3) . 2_655
P2 Re2 P2 158.05(6) . 2_655
Re1 Re2 Br2 114.034(14) . 2_655
P2 Re2 Br2 85.43(3) . 2_655
P2 Re2 Br2 85.67(3) 2_655 2_655
Re1 Re2 Br2 114.035(14) . .
P2 Re2 Br2 85.67(3) . .
P2 Re2 Br2 85.43(3) 2_655 .
Br2 Re2 Br2 131.93(3) 2_655 .
C3 P1 C2 102.5(3) . .
C3 P1 C1 102.3(3) . .
C2 P1 C1 101.5(3) . .
C3 P1 Re1 119.10(18) . .
C2 P1 Re1 121.03(18) . .
C1 P1 Re1 107.6(2) . .
C5 P2 C6 102.0(3) . .
C5 P2 C4 102.4(3) . .
C6 P2 C4 102.0(3) . .
C5 P2 Re2 119.70(19) . .
C6 P2 Re2 107.65(19) . .
C4 P2 Re2 120.30(19) . .
P1 C1 H1A 109.5 . .
P1 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
P1 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
P1 C2 H2A 109.5 . .
P1 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
P1 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
P1 C3 H3A 109.5 . .
P1 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
P1 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
P2 C4 H4A 109.5 . .
P2 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
P2 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
P2 C5 H5A 109.5 . .
P2 C5 H5B 109.5 . .
H5A C5 H5B 109.5 . .
P2 C5 H5C 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
P2 C6 H6A 109.5 . .
P2 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
P2 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Re1 Re2 2.2521(3) .
Re1 P1 2.4181(11) 2_655
Re1 P1 2.4181(11) .
Re1 Br1 2.5025(5) 2_655
Re1 Br1 2.5025(5) .
Re2 P2 2.4210(11) .
Re2 P2 2.4210(11) 2_655
Re2 Br2 2.5051(5) 2_655
Re2 Br2 2.5051(5) .
P1 C3 1.815(5) .
P1 C2 1.816(5) .
P1 C1 1.826(5) .
P2 C5 1.815(6) .
P2 C6 1.823(5) .
P2 C4 1.830(5) .
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
C3 H3A 0.9800 .
C3 H3B 0.9800 .
C3 H3C 0.9800 .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C4 H4C 0.9800 .
C5 H5A 0.9800 .
C5 H5B 0.9800 .
C5 H5C 0.9800 .
C6 H6A 0.9800 .
C6 H6B 0.9800 .
C6 H6C 0.9800 .
