#------------------------------------------------------------------------------
#$Date: 2015-06-16 09:52:12 +0300 (Tue, 16 Jun 2015) $
#$Revision: 139251 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/07/7220771.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_7220771
loop_
_publ_author_name
'Martinez-Lillo, Jose'
'Armentano, Donatella'
_publ_section_title
;
 Aquapentachlororhenate(IV): a singular and promising building block for
 metal assembling
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA10225A
_journal_year                    2015
_chemical_formula_sum            'C24 H22 Cl5 O P Re'
_chemical_formula_weight         720.83
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           85
_space_group_name_Hall           '-P 4a'
_space_group_name_H-M_alt        'P 4/n'
_symmetry_space_group_name_Hall  '-P 4a'
_symmetry_space_group_name_H-M   'P 4/n :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-02-17 deposited with the CCDC.
2015-06-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.3512(11)
_cell_length_b                   13.3512(11)
_cell_length_c                   7.2677(8)
_cell_measurement_reflns_used    9853
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.57
_cell_measurement_theta_min      3.05
_cell_volume                     1295.5(2)
_computing_cell_refinement       'Bruker APEX'
_computing_data_collection       'Bruker APEX'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0206
_diffrn_reflns_av_unetI/netI     0.0092
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            15280
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.979
_diffrn_reflns_theta_min         2.157
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    5.283
_exptl_absorpt_correction_T_max  0.602
_exptl_absorpt_correction_T_min  0.420
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.848
_exptl_crystal_description       irregular
_exptl_crystal_F_000             698
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile:water (9:1, v/v) solution '
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         4.579
_refine_diff_density_min         -0.793
_refine_diff_density_rms         0.420
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.280
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     75
_refine_ls_number_reflns         1425
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.280
_refine_ls_R_factor_all          0.0813
_refine_ls_R_factor_gt           0.0804
_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)+(0.1916P)²+3.3997P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2639
_refine_ls_wR_factor_ref         0.2665
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1381
_reflns_number_total             1425
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5ra10225a2.cif
_cod_data_source_block           repyzmo
_cod_original_cell_volume        1295.5(3)
_cod_database_code               7220771
_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.
;
_shelxl_version_number           2013-4
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-y+1/2, x, z'
'y, -x+1/2, z'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y-1/2, -x, -z'
'-y, x-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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Re1 Re 0.2500 0.2500 0.36663(9) 0.0379(5) Uani 1 4 d S T P
Cl1 Cl 0.4133(2) 0.1928(2) 0.3568(3) 0.0430(7) Uani 1 1 d . . .
Cl2 Cl 0.2500 0.2500 0.0480(8) 0.0556(14) Uani 1 4 d S T P
O1W O 0.2500 0.2500 0.6492(18) 0.042(4) Uani 1 4 d S T P
P1 P 0.7500 0.2500 0.5000 0.0340(10) Uani 1 4 d S T P
C1 C 0.6541(8) 0.2032(8) 0.6452(11) 0.035(2) Uani 1 1 d . . .
C2 C 0.6177(9) 0.2660(8) 0.7803(14) 0.050(3) Uani 1 1 d . . .
H2 H 0.6425 0.3308 0.7914 0.060 Uiso 1 1 calc R U .
C3 C 0.5441(13) 0.2320(11) 0.8992(17) 0.059(4) Uani 1 1 d . . .
H3 H 0.5172 0.2737 0.9891 0.071 Uiso 1 1 calc R U .
C4 C 0.5127(15) 0.1370(12) 0.8806(16) 0.061(4) Uani 1 1 d . . .
H4 H 0.4654 0.1129 0.9634 0.073 Uiso 1 1 calc R U .
C5 C 0.5465(10) 0.0742(8) 0.7470(17) 0.051(2) Uani 1 1 d . . .
H5 H 0.5199 0.0102 0.7347 0.061 Uiso 1 1 calc R U .
C6 C 0.6196(9) 0.1068(8) 0.6321(11) 0.036(2) Uani 1 1 d . . .
H6 H 0.6463 0.0638 0.5443 0.043 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'
Cl Cl 0.1484 0.1585 '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'
O O 0.0106 0.0060 '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
O1W Re1 Cl1 91.78(6) . .
O1W Re1 Cl1 91.78(6) . 4
Cl1 Re1 Cl1 89.946(4) . 4
O1W Re1 Cl1 91.78(6) . 3
Cl1 Re1 Cl1 89.944(4) . 3
Cl1 Re1 Cl1 176.44(12) 4 3
O1W Re1 Cl1 91.78(6) . 2
Cl1 Re1 Cl1 176.44(12) . 2
Cl1 Re1 Cl1 89.945(4) 4 2
Cl1 Re1 Cl1 89.945(4) 3 2
O1W Re1 Cl2 180.0 . .
Cl1 Re1 Cl2 88.22(6) . .
Cl1 Re1 Cl2 88.22(6) 4 .
Cl1 Re1 Cl2 88.22(6) 3 .
Cl1 Re1 Cl2 88.22(6) 2 .
C1 P1 C1 106.9(6) . 2_655
C1 P1 C1 110.8(3) . 8_656
C1 P1 C1 110.8(3) 2_655 8_656
C1 P1 C1 110.8(3) . 7_666
C1 P1 C1 110.8(3) 2_655 7_666
C1 P1 C1 106.9(6) 8_656 7_666
C6 C1 C2 120.2(9) . .
C6 C1 P1 122.1(8) . .
C2 C1 P1 117.6(8) . .
C1 C2 C3 119.7(10) . .
C4 C3 C2 117.9(12) . .
C3 C4 C5 123.4(12) . .
C6 C5 C4 118.7(10) . .
C5 C6 C1 120.0(10) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Re1 O1W 2.054(13) .
Re1 Cl1 2.311(3) .
Re1 Cl1 2.311(3) 4
Re1 Cl1 2.311(3) 3
Re1 Cl1 2.311(3) 2
Re1 Cl2 2.315(6) .
P1 C1 1.773(10) .
P1 C1 1.773(10) 2_655
P1 C1 1.773(10) 8_656
P1 C1 1.773(10) 7_666
C1 C6 1.370(15) .
C1 C2 1.379(14) .
C2 C3 1.386(16) .
C3 C4 1.34(2) .
C4 C5 1.36(2) .
C5 C6 1.357(16) .
