Temperature and Solvent Effects on H<sub>2</sub> Splitting and Hydricity: Ramifications on CO<sub>2</sub> Hydrogenation by a Rhenium Pincer Catalyst.
Hu, Jenny; Bruch, Quinton J.; Miller, Alexander J. M.; Journal of the American Chemical Society 143 (2021) 945–954; doi:10.1021/jacs.0c11110

data_4135498
_publ_section_title
;
 Temperature and Solvent Effects on H<sub>2</sub> Splitting and Hydricity:
 Ramifications on CO<sub>2</sub> 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         'C25 H39 O5 P2 Re'
_chemical_formula_sum            'C25 H39 O5 P2 Re'
_chemical_formula_weight         667.70
_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)
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_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       '\f and \w 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
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_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.4233
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_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 \l/2 correction factor is Not present.'
_exptl_crystal_colour            orange
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_refine_ls_number_reflns         4839
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_refine_ls_restrained_S_all      1.164
_refine_ls_R_factor_all          0.0232
_refine_ls_R_factor_gt           0.0225
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0295P)^2^+1.3712P] where P=(Fo^2^+2Fc^2^)/3'
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_reflns_number_gt                4734
_reflns_number_total             4839
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c11110_si_004.cif
_cod_data_source_block           x1806002
_cod_depositor_comments
;
Adding full bibliography for 4135498--4135499.cif.

2025-09-12
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C50 H78 O10 P4 Re2'
_cod_original_formula_weight         1335.40
_cod_original_formula_moiety         '2(C25 H39 O5 P2 Re)'
_cod_original_formula_units_Z            1
_cod_original_cell_volume        1361.8(17)
_cod_database_code               4135498
_shelx_shelxl_version_number     2018/3
_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)
;
_shelx_res_checksum              78756
_shelx_hkl_checksum              52131
_olex2_submission_special_instructions 'No special instructions were received'