#------------------------------------------------------------------------------
#$Date: 2019-11-17 11:12:28 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229515 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/75/7047586.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_7047586
loop_
_publ_author_name
'Arumugam, Ramar'
'Shankar, Bhaskaran'
'Shanmugam, Ramasamy'
'Arumuganathan, T.'
'Sathiyendiran, Malaichamy'
_publ_section_title
;
 Phosphine oxide-based tricarbonylrhenium(i) complexes from
 phosphine/phosphine oxide and dihydroxybenzoquinones.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13894
_journal_page_last               13901
_journal_paper_doi               10.1039/c8dt02985g
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C48 H32 O12 P2 Re2'
_chemical_formula_sum            'C48 H32 O12 P2 Re2'
_chemical_formula_weight         1235.07
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2018-08-26 deposited with the CCDC.
2018-09-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.377(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.052(3)
_cell_length_b                   9.4296(10)
_cell_length_c                   26.152(3)
_cell_measurement_reflns_used    9946
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.67
_cell_measurement_theta_min      2.35
_cell_volume                     5425.2(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_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  0.1561
_diffrn_reflns_av_unetI/netI     0.0699
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            67528
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.212
_diffrn_reflns_theta_min         2.350
_exptl_absorpt_coefficient_mu    4.570
_exptl_absorpt_correction_T_max  0.804
_exptl_absorpt_correction_T_min  0.711
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   multi-scan
_exptl_crystal_colour            'Dark red'
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_description       Needle
_exptl_crystal_F_000             2384
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.075
_refine_diff_density_min         -0.924
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         6004
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.1153
_refine_ls_R_factor_gt           0.0507
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0427P)²+33.4737P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1036
_refine_ls_wR_factor_ref         0.1259
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3440
_reflns_number_total             6004
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8dt02985g2.cif
_cod_data_source_block           Compound_2
_cod_depositor_comments
'Adding full bibliography for 7047584--7047588.cif.'
_cod_original_cell_volume        5425.1(11)
_cod_database_code               7047586
_shelx_shelxl_version_number     2018/3
_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.
;
_shelx_estimated_absorpt_t_min   0.711
_shelx_estimated_absorpt_t_max   0.804
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
Re1 Re 0.23354(2) 0.39974(4) 0.40805(2) 0.06158(14) Uani 1 1 d . .
P1 P 0.35960(11) 0.4989(2) 0.37299(8) 0.0543(5) Uani 1 1 d . .
O5 O 0.2734(3) 0.4769(6) 0.4881(2) 0.0648(15) Uani 1 1 d . .
O4 O 0.3091(3) 0.5164(6) 0.3978(2) 0.0674(16) Uani 1 1 d . .
O6 O 0.2005(3) 0.6115(7) 0.4075(2) 0.0689(16) Uani 1 1 d . .
O3 O 0.2904(4) 0.1053(8) 0.4215(3) 0.106(3) Uani 1 1 d . .
O2 O 0.1741(4) 0.3330(8) 0.2903(3) 0.103(2) Uani 1 1 d . .
C22 C 0.2647(4) 0.6070(9) 0.4964(3) 0.0546(19) Uani 1 1 d . .
C4 C 0.3361(4) 0.4129(8) 0.3093(3) 0.0536(19) Uani 1 1 d . .
C2 C 0.1973(5) 0.3577(9) 0.3347(4) 0.078(3) Uani 1 1 d . .
C10 C 0.4210(4) 0.3959(9) 0.4147(3) 0.061(2) Uani 1 1 d . .
C8 C 0.3192(5) 0.2012(10) 0.2572(4) 0.080(3) Uani 1 1 d . .
H8 H 0.322090 0.103006 0.255515 0.096 Uiso 1 1 calc R U
C23 C 0.2219(4) 0.6854(9) 0.4498(3) 0.057(2) Uani 1 1 d . .
C21 C 0.3702(4) 0.7892(9) 0.3883(3) 0.069(2) Uani 1 1 d . .
H21 H 0.340964 0.780022 0.406065 0.082 Uiso 1 1 calc R U
C9 C 0.3405(4) 0.2698(9) 0.3049(3) 0.067(2) Uani 1 1 d . .
H9 H 0.358660 0.217100 0.335562 0.080 Uiso 1 1 calc R U
C3 C 0.2690(5) 0.2158(12) 0.4159(4) 0.083(3) Uani 1 1 d . .
O1 O 0.1248(4) 0.2695(12) 0.4311(4) 0.142(4) Uani 1 1 d . .
C16 C 0.3878(4) 0.6721(8) 0.3646(3) 0.056(2) Uani 1 1 d . .
C5 C 0.3097(4) 0.4932(10) 0.2632(3) 0.065(2) Uani 1 1 d . .
H5 H 0.307161 0.591340 0.265114 0.078 Uiso 1 1 calc R U
C11 C 0.4691(5) 0.3534(10) 0.3960(4) 0.083(3) Uani 1 1 d . .
H11 H 0.468511 0.375726 0.361207 0.100 Uiso 1 1 calc R U
C6 C 0.2873(5) 0.4233(13) 0.2143(4) 0.088(3) Uani 1 1 d . .
H6 H 0.268338 0.474695 0.183476 0.106 Uiso 1 1 calc R U
C24 C 0.2908(4) 0.6741(9) 0.5447(3) 0.065(2) Uani 1 1 d . .
H24 H 0.316823 0.624793 0.573233 0.078 Uiso 1 1 calc R U
C7 C 0.2932(5) 0.2786(14) 0.2114(4) 0.089(3) Uani 1 1 d . .
H7 H 0.279611 0.232922 0.178501 0.106 Uiso 1 1 calc R U
C17 C 0.4316(5) 0.6901(11) 0.3398(4) 0.092(3) Uani 1 1 d . .
H17 H 0.444841 0.612144 0.324522 0.111 Uiso 1 1 calc R U
C15 C 0.4212(5) 0.3652(11) 0.4657(3) 0.083(3) Uani 1 1 d . .
H15 H 0.389164 0.394914 0.477933 0.100 Uiso 1 1 calc R U
C1 C 0.1672(5) 0.3180(13) 0.4232(4) 0.088(3) Uani 1 1 d . .
C12 C 0.5170(5) 0.2794(13) 0.4285(5) 0.102(4) Uani 1 1 d . .
H12 H 0.549219 0.251180 0.416349 0.122 Uiso 1 1 calc R U
C20 C 0.3963(5) 0.9196(10) 0.3854(4) 0.088(3) Uani 1 1 d . .
H20 H 0.384442 0.998631 0.400996 0.105 Uiso 1 1 calc R U
C19 C 0.4392(6) 0.9328(10) 0.3598(5) 0.099(4) Uani 1 1 d . .
H19 H 0.456866 1.020727 0.358171 0.119 Uiso 1 1 calc R U
C18 C 0.4564(6) 0.8192(11) 0.3368(5) 0.109(4) Uani 1 1 d . .
H18 H 0.485374 0.829231 0.318830 0.130 Uiso 1 1 calc R U
C14 C 0.4691(7) 0.2899(16) 0.4993(4) 0.116(5) Uani 1 1 d . .
H14 H 0.469494 0.268189 0.534144 0.139 Uiso 1 1 calc R U
C13 C 0.5162(7) 0.2474(15) 0.4804(6) 0.126(5) Uani 1 1 d . .
H13 H 0.548276 0.196137 0.502847 0.151 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'
O O 0.0106 0.0060 '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'
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
C1 Re1 C2 89.2(4) . .
C1 Re1 C3 87.4(5) . .
C2 Re1 C3 87.9(4) . .
C1 Re1 O6 94.3(4) . .
C2 Re1 O6 98.1(3) . .
C3 Re1 O6 173.8(3) . .
C1 Re1 O4 172.3(4) . .
C2 Re1 O4 96.3(3) . .
C3 Re1 O4 98.2(4) . .
O6 Re1 O4 79.7(2) . .
C1 Re1 O5 94.2(3) . .
C2 Re1 O5 172.3(3) . .
C3 Re1 O5 99.1(3) . .
O6 Re1 O5 74.8(2) . .
O4 Re1 O5 79.6(2) . .
O4 P1 C4 113.3(4) . .
O4 P1 C10 111.7(4) . .
C4 P1 C10 106.6(4) . .
O4 P1 C16 108.0(4) . .
C4 P1 C16 108.6(4) . .
C10 P1 C16 108.5(4) . .
C22 O5 Re1 116.7(5) . .
P1 O4 Re1 139.6(3) . .
C23 O6 Re1 117.5(5) . .
O5 C22 C24 123.4(7) . .
O5 C22 C23 115.6(7) . .
C24 C22 C23 121.0(8) . .
C9 C4 C5 119.2(7) . .
C9 C4 P1 121.3(6) . .
C5 C4 P1 119.4(6) . .
O2 C2 Re1 178.5(10) . .
C15 C10 C11 120.8(9) . .
C15 C10 P1 118.8(8) . .
C11 C10 P1 120.4(6) . .
C9 C8 C7 119.3(9) . .
O6 C23 C24 125.4(8) . 7_566
O6 C23 C22 114.9(7) . .
C24 C23 C22 119.7(7) 7_566 .
C20 C21 C16 119.6(9) . .
C8 C9 C4 122.3(9) . .
O3 C3 Re1 178.8(8) . .
C17 C16 C21 118.1(8) . .
C17 C16 P1 121.2(7) . .
C21 C16 P1 120.3(7) . .
C6 C5 C4 118.8(9) . .
C12 C11 C10 120.4(10) . .
C7 C6 C5 120.2(9) . .
C23 C24 C22 119.3(7) 7_566 .
C6 C7 C8 120.2(9) . .
C18 C17 C16 121.5(10) . .
C10 C15 C14 119.9(11) . .
O1 C1 Re1 177.7(11) . .
C11 C12 C13 118.2(12) . .
C19 C20 C21 120.3(9) . .
C18 C19 C20 120.2(10) . .
C19 C18 C17 120.3(11) . .
C13 C14 C15 119.0(11) . .
C14 C13 C12 121.7(12) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Re1 C1 1.858(12) .
Re1 C2 1.892(11) .
Re1 C3 1.902(12) .
Re1 O6 2.135(6) .
Re1 O4 2.144(6) .
Re1 O5 2.146(5) .
P1 O4 1.502(6) .
P1 C4 1.785(7) .
P1 C10 1.794(9) .
P1 C16 1.796(8) .
O5 C22 1.272(9) .
O6 C23 1.275(9) .
O3 C3 1.144(12) .
O2 C2 1.147(11) .
C22 C24 1.380(11) .
C22 C23 1.513(11) .
C4 C9 1.361(11) .
C4 C5 1.400(11) .
C10 C15 1.364(11) .
C10 C11 1.397(13) .
C8 C9 1.360(12) .
C8 C7 1.377(14) .
C23 C24 1.373(12) 7_566
C21 C20 1.382(13) .
C21 C16 1.385(11) .
O1 C1 1.150(12) .
C16 C17 1.364(12) .
C5 C6 1.393(12) .
C11 C12 1.366(14) .
C6 C7 1.376(15) .
C17 C18 1.356(14) .
C15 C14 1.384(16) .
C12 C13 1.397(17) .
C20 C19 1.354(15) .
C19 C18 1.344(15) .
C14 C13 1.381(17) .
