#------------------------------------------------------------------------------
#$Date: 2021-02-04 05:30:21 +0200 (Thu, 04 Feb 2021) $
#$Revision: 261499 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/54/4135498.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_4135498
loop_
_publ_author_name
'Hu, Jenny'
'Bruch, Quinton J.'
'Miller, Alexander J. M.'
_publ_section_title
;
 Temperature and Solvent Effects on H₂ Splitting and Hydricity:
 Ramifications on CO₂ Hydrogenation by a Rhenium Pincer
 Catalyst.
;
_journal_issue                   2
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              945
_journal_page_last               954
_journal_paper_doi               10.1021/jacs.0c11110
_journal_volume                  143
_journal_year                    2021
_chemical_formula_moiety         '2(C25 H39 O5 P2 Re)'
_chemical_formula_sum            'C50 H78 O10 P4 Re2'
_chemical_formula_weight         1335.40
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-07-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                98.51(2)
_cell_angle_beta                 98.60(4)
_cell_angle_gamma                105.218(15)
_cell_formula_units_Z            1
_cell_length_a                   8.677(7)
_cell_length_b                   12.469(8)
_cell_length_c                   13.453(10)
_cell_measurement_reflns_used    9629
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.356
_cell_measurement_theta_min      3.393
_cell_volume                     1361.7(17)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            26212
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.155
_diffrn_reflns_theta_min         3.388
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.098
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.4233
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1150 before and 0.0493 after correction. The Ratio of minimum to maximum transmission is 0.5621. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.628
_exptl_crystal_description       plate
_exptl_crystal_F_000             668
_refine_diff_density_max         1.373
_refine_diff_density_min         -0.601
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.164
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         4839
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.164
_refine_ls_R_factor_all          0.0232
_refine_ls_R_factor_gt           0.0225
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0295P)²+1.3712P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0563
_refine_ls_wR_factor_ref         0.0566
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4734
_reflns_number_total             4839
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja0c11110_si_004.cif
_cod_data_source_block           x1806002
_cod_depositor_comments
'Adding full bibliography for 4135498--4135499.cif.'
_cod_original_cell_volume        1361.8(17)
_cod_database_code               4135498
_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.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C4(H4), C3(H3)
2.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C13(H13A,H13B,H13C),
 C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C12(H12A,H12B,
 H12C), C21(H21A,H21B,H21C), C20(H20A,H20B,H20C), C18(H18A,H18B,H18C), C22(H22A,
 H22B,H22C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Re1 Re 0.59824(2) 0.71493(2) 0.77032(2) 0.01197(6) Uani 1 1 d . . . . .
P2 P 0.72311(9) 0.90260(6) 0.73795(5) 0.01271(14) Uani 1 1 d . . . . .
P1 P 0.36492(9) 0.54744(6) 0.74304(6) 0.01462(15) Uani 1 1 d . . . . .
O1 O 0.2557(3) 0.54385(17) 0.63029(16) 0.0178(4) Uani 1 1 d . . . . .
O2 O 0.6142(2) 0.90888(17) 0.62791(16) 0.0159(4) Uani 1 1 d . . . . .
O3 O 0.4993(3) 0.8205(2) 0.96656(19) 0.0313(6) Uani 1 1 d . . . . .
O4 O 0.8482(3) 0.6758(2) 0.9414(2) 0.0329(6) Uani 1 1 d . . . . .
O5 O 0.7337(4) 0.5972(2) 0.5930(2) 0.0344(6) Uani 1 1 d . . . . .
C1 C 0.4314(4) 0.7313(2) 0.6396(2) 0.0139(6) Uani 1 1 d . . . . .
C24 C 0.7573(4) 0.6900(3) 0.8762(2) 0.0198(6) Uani 1 1 d . . . . .
C6 C 0.4668(4) 0.8234(2) 0.5907(2) 0.0143(6) Uani 1 1 d . . . . .
C5 C 0.3654(4) 0.8343(3) 0.5051(2) 0.0172(6) Uani 1 1 d . . . . .
H5 H 0.392248 0.899538 0.475292 0.021 Uiso 1 1 calc R . . . .
C4 C 0.2231(4) 0.7463(3) 0.4643(2) 0.0190(6) Uani 1 1 d . . . . .
H4 H 0.150415 0.752726 0.406755 0.023 Uiso 1 1 calc R . . . .
C25 C 0.6854(4) 0.6404(3) 0.6588(3) 0.0226(7) Uani 1 1 d . . . . .
C11 C 0.9340(4) 0.9460(3) 0.7087(2) 0.0180(6) Uani 1 1 d . . . . .
C3 C 0.1848(4) 0.6494(3) 0.5058(2) 0.0177(6) Uani 1 1 d . . . . .
H3 H 0.088837 0.588820 0.476655 0.021 Uiso 1 1 calc R . . . .
C8 C 0.5040(4) 1.0048(3) 0.8082(3) 0.0209(6) Uani 1 1 d . . . . .
H8A H 0.461625 1.015175 0.739739 0.031 Uiso 1 1 calc GR . . . .
H8B H 0.478906 1.058025 0.860147 0.031 Uiso 1 1 calc GR . . . .
H8C H 0.453246 0.926962 0.815350 0.031 Uiso 1 1 calc GR . . . .
C9 C 0.7691(4) 1.0350(3) 0.9361(2) 0.0214(6) Uani 1 1 d . . . . .
H9A H 0.763106 0.958650 0.948629 0.032 Uiso 1 1 calc GR . . . .
H9B H 0.709852 1.070260 0.981317 0.032 Uiso 1 1 calc GR . . . .
H9C H 0.883335 1.080848 0.950083 0.032 Uiso 1 1 calc GR . . . .
C7 C 0.6918(4) 1.0272(3) 0.8233(2) 0.0170(6) Uani 1 1 d . . . . .
C15 C 0.2063(4) 0.5556(3) 0.8240(2) 0.0214(7) Uani 1 1 d . . . . .
C2 C 0.2915(4) 0.6440(2) 0.5914(2) 0.0150(6) Uani 1 1 d . . . . .
C23 C 0.5278(4) 0.7834(3) 0.8897(3) 0.0199(6) Uani 1 1 d . . . . .
C10 C 0.7574(4) 1.1426(3) 0.7943(3) 0.0255(7) Uani 1 1 d . . . . .
H10A H 0.876684 1.163752 0.806538 0.038 Uiso 1 1 calc GR . . . .
H10B H 0.723108 1.199963 0.836249 0.038 Uiso 1 1 calc GR . . . .
H10C H 0.714485 1.137995 0.721679 0.038 Uiso 1 1 calc GR . . . .
C13 C 1.0599(4) 0.9916(3) 0.8093(3) 0.0321(8) Uani 1 1 d . . . . .
H13A H 1.047556 1.063057 0.843382 0.048 Uiso 1 1 calc GR . . . .
H13B H 1.169827 1.004621 0.794528 0.048 Uiso 1 1 calc GR . . . .
H13C H 1.042722 0.936167 0.854149 0.048 Uiso 1 1 calc GR . . . .
C19 C 0.3856(4) 0.3994(3) 0.7232(3) 0.0241(7) Uani 1 1 d . . . . .
C14 C 0.9686(4) 0.8413(3) 0.6514(3) 0.0277(7) Uani 1 1 d . . . . .
H14A H 0.971352 0.786724 0.696648 0.042 Uiso 1 1 calc GR . . . .
H14B H 1.074000 0.864335 0.630498 0.042 Uiso 1 1 calc GR . . . .
H14C H 0.882547 0.805987 0.590481 0.042 Uiso 1 1 calc GR . . . .
C16 C 0.2767(5) 0.5677(3) 0.9387(3) 0.0311(8) Uani 1 1 d . . . . .
H16A H 0.267672 0.492366 0.954701 0.047 Uiso 1 1 calc GR . . . .
H16B H 0.215486 0.605763 0.980181 0.047 Uiso 1 1 calc GR . . . .
H16C H 0.391489 0.612596 0.954240 0.047 Uiso 1 1 calc GR . . . .
C17 C 0.1513(4) 0.6601(3) 0.8040(3) 0.0267(7) Uani 1 1 d . . . . .
H17A H 0.247259 0.724079 0.807311 0.040 Uiso 1 1 calc GR . . . .
H17B H 0.090519 0.680237 0.856064 0.040 Uiso 1 1 calc GR . . . .
H17C H 0.081379 0.642340 0.735845 0.040 Uiso 1 1 calc GR . . . .
C12 C 0.9539(4) 1.0331(3) 0.6383(3) 0.0263(7) Uani 1 1 d . . . . .
H12A H 0.869503 1.003887 0.575780 0.039 Uiso 1 1 calc GR . . . .
H12B H 1.061638 1.046505 0.620076 0.039 Uiso 1 1 calc GR . . . .
H12C H 0.943150 1.104378 0.673975 0.039 Uiso 1 1 calc GR . . . .
C21 C 0.2350(5) 0.3123(3) 0.6523(3) 0.0314(8) Uani 1 1 d . . . . .
H21A H 0.141435 0.303836 0.686363 0.047 Uiso 1 1 calc GR . . . .
H21B H 0.257032 0.239019 0.637276 0.047 Uiso 1 1 calc GR . . . .
H21C H 0.210772 0.338552 0.588254 0.047 Uiso 1 1 calc GR . . . .
C20 C 0.4152(5) 0.3650(3) 0.8281(3) 0.0372(9) Uani 1 1 d . . . . .
H20A H 0.505101 0.424163 0.874655 0.056 Uiso 1 1 calc GR . . . .
H20B H 0.443023 0.293370 0.819569 0.056 Uiso 1 1 calc GR . . . .
H20C H 0.316235 0.355545 0.856886 0.056 Uiso 1 1 calc GR . . . .
C18 C 0.0499(4) 0.4548(3) 0.7939(3) 0.0310(8) Uani 1 1 d . . . . .
H18A H 0.010050 0.440198 0.719646 0.047 Uiso 1 1 calc GR . . . .
H18B H -0.033471 0.472703 0.829505 0.047 Uiso 1 1 calc GR . . . .
H18C H 0.073824 0.387278 0.813380 0.047 Uiso 1 1 calc GR . . . .
C22 C 0.5318(5) 0.3968(3) 0.6728(4) 0.0364(9) Uani 1 1 d . . . . .
H22A H 0.516739 0.421741 0.607213 0.055 Uiso 1 1 calc GR . . . .
H22B H 0.540780 0.319453 0.660978 0.055 Uiso 1 1 calc GR . . . .
H22C H 0.631457 0.447710 0.717988 0.055 Uiso 1 1 calc GR . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -5.2083 5.8923 '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
_geom_angle_publ_flag
P1 Re1 P2 150.39(3) . . ?
C1 Re1 P2 75.61(9) . . ?
C1 Re1 P1 75.55(9) . . ?
C24 Re1 P2 105.45(10) . . ?
C24 Re1 P1 103.97(11) . . ?
C24 Re1 C1 173.43(12) . . ?
C24 Re1 C25 91.91(15) . . ?
C24 Re1 C23 82.30(14) . . ?
C25 Re1 P2 91.78(10) . . ?
C25 Re1 P1 90.53(11) . . ?
C25 Re1 C1 81.56(13) . . ?
C23 Re1 P2 90.37(10) . . ?
C23 Re1 P1 90.26(10) . . ?
C23 Re1 C1 104.23(13) . . ?
C23 Re1 C25 174.17(13) . . ?
O2 P2 Re1 105.17(8) . . ?
O2 P2 C11 99.88(14) . . ?
O2 P2 C7 99.16(13) . . ?
C11 P2 Re1 122.87(10) . . ?
C11 P2 C7 108.73(14) . . ?
C7 P2 Re1 116.55(11) . . ?
O1 P1 Re1 105.03(9) . . ?
O1 P1 C15 98.67(14) . . ?
O1 P1 C19 100.24(14) . . ?
C15 P1 Re1 116.71(11) . . ?
C19 P1 Re1 122.34(12) . . ?
C19 P1 C15 109.29(15) . . ?
C2 O1 P1 116.42(18) . . ?
C6 O2 P2 116.81(19) . . ?
C6 C1 Re1 122.4(2) . . ?
C2 C1 Re1 122.0(2) . . ?
C2 C1 C6 115.2(3) . . ?
O4 C24 Re1 177.6(3) . . ?
C1 C6 O2 118.8(3) . . ?
C5 C6 O2 117.5(3) . . ?
C5 C6 C1 123.7(3) . . ?
C6 C5 C4 117.7(3) . . ?
C3 C4 C5 121.5(3) . . ?
O5 C25 Re1 178.9(3) . . ?
C13 C11 P2 109.5(2) . . ?
C13 C11 C14 108.2(3) . . ?
C13 C11 C12 110.7(3) . . ?
C14 C11 P2 109.0(2) . . ?
C12 C11 P2 113.1(2) . . ?
C12 C11 C14 106.2(3) . . ?
C2 C3 C4 117.7(3) . . ?
C8 C7 P2 105.4(2) . . ?
C9 C7 P2 110.5(2) . . ?
C9 C7 C8 111.5(3) . . ?
C10 C7 P2 115.2(2) . . ?
C10 C7 C8 105.7(3) . . ?
C10 C7 C9 108.4(3) . . ?
C16 C15 P1 111.4(2) . . ?
C16 C15 C17 111.1(3) . . ?
C17 C15 P1 105.8(2) . . ?
C18 C15 P1 114.9(2) . . ?
C18 C15 C16 108.2(3) . . ?
C18 C15 C17 105.4(3) . . ?
C1 C2 O1 118.7(3) . . ?
C3 C2 O1 117.4(3) . . ?
C3 C2 C1 123.8(3) . . ?
O3 C23 Re1 172.5(3) . . ?
C21 C19 P1 112.5(2) . . ?
C20 C19 P1 109.1(2) . . ?
C20 C19 C21 110.0(3) . . ?
C22 C19 P1 109.5(2) . . ?
C22 C19 C21 107.0(3) . . ?
C22 C19 C20 108.6(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Re1 P2 2.4395(15) . ?
Re1 P1 2.4344(15) . ?
Re1 C1 2.175(3) . ?
Re1 C24 1.950(3) . ?
Re1 C25 1.995(4) . ?
Re1 C23 1.961(4) . ?
P2 O2 1.657(2) . ?
P2 C11 1.885(3) . ?
P2 C7 1.896(3) . ?
P1 O1 1.652(2) . ?
P1 C15 1.892(4) . ?
P1 C19 1.885(3) . ?
O1 C2 1.403(4) . ?
O2 C6 1.399(4) . ?
O3 C23 1.157(4) . ?
O4 C24 1.155(4) . ?
O5 C25 1.157(4) . ?
C1 C6 1.394(4) . ?
C1 C2 1.393(4) . ?
C6 C5 1.388(4) . ?
C5 C4 1.392(4) . ?
C4 C3 1.388(4) . ?
C11 C13 1.533(5) . ?
C11 C14 1.539(4) . ?
C11 C12 1.537(4) . ?
C3 C2 1.387(4) . ?
C8 C7 1.555(4) . ?
C9 C7 1.544(4) . ?
C7 C10 1.532(5) . ?
C15 C16 1.543(5) . ?
C15 C17 1.546(5) . ?
C15 C18 1.541(5) . ?
C19 C21 1.540(5) . ?
C19 C20 1.539(5) . ?
C19 C22 1.531(5) . ?
