Tuning Catalytic Activity in the Hydrogenation of Unactivated Olefins with Transition-Metal Oxos as the Lewis Base Component of Frustrated Lewis Pairs
Lambic, Nikola S.; Sommer, Roger D.; Ison, Elon A.; ACS Catalysis 7 (2017) 1170–; doi:10.1021/acscatal.6b03313

data_4514011
_publ_section_title
;
 Tuning Catalytic Activity in the Hydrogenation of Unactivated Olefins
 with Transition-Metal Oxos as the Lewis Base Component of Frustrated
 Lewis Pairs
;
_journal_issue                   2
_journal_name_full               'ACS Catalysis'
_journal_page_first              1170
_journal_paper_doi               10.1021/acscatal.6b03313
_journal_volume                  7
_journal_year                    2017
_chemical_formula_moiety         'C37 H46 N3 O Re, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C37.5 H47 Cl N3 O Re'
_chemical_formula_weight         777.43
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2016-12-09
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_cell_angle_alpha                90
_cell_angle_beta                 105.914(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.6648(7)
_cell_length_b                   13.4862(5)
_cell_length_c                   17.0820(8)
_cell_measurement_reflns_used    9890
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.06
_cell_measurement_theta_min      2.48
_cell_volume                     3470.4(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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      100.02
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 8
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            37598
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.124
_diffrn_reflns_theta_max         25.124
_diffrn_reflns_theta_min         1.954
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.611
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5720
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0705 before and 0.0414 after correction. The Ratio of minimum to maximum transmission is 0.7676. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_description       plate
_exptl_crystal_F_000             1572
_exptl_crystal_recrystallization_method
'Vapor Diffusion methylene chloride/ pentane'
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.022
_refine_diff_density_min         -0.804
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     414
_refine_ls_number_reflns         6169
_refine_ls_number_restraints     41
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0203
_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/[\s^2^(Fo^2^)+(0.0167P)^2^+5.2998P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0427
_refine_ls_wR_factor_ref         0.0458
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5231
_reflns_number_total             6169
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs6b03313_si_002.cif
_cod_data_source_block           rds398_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to
/usr/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 
;
_cod_original_formula_sum        'C37.50 H47 Cl N3 O Re'
_cod_database_code               4514011
_shelx_estimated_absorpt_t_max   0.737
_shelx_estimated_absorpt_t_min   0.504
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C1S-Cl1S
 1.74 with sigma of 0.02
 C1S-Cl2S
 1.74 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C1S \\sim Cl2S \\sim Cl1S: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Uanis(Cl2S) \\sim Ueq, Uanis(C1S) \\sim Ueq, Uanis(Cl1S) \\sim Ueq: with sigma
of 0.1 and sigma for terminal atoms of 0.2
4. Rigid body (RIGU) restrains
 Cl2S, C1S, Cl1S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: Cl1S(0.5) Cl2S(0.5) C1S(0.5) H1SA(0.5) H1SB(0.5)
6.a Ternary CH refined with riding coordinates:
 C35(H35), C20(H20), C32(H32), C23(H23)
6.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C7(H7A,H7B), C1S(H1SA,H1SB)
6.c Aromatic/amide H refined with riding coordinates:
 C28(H28), C6(H6), C10(H10), C29(H29), C2(H2), C30(H30), C11(H11), C9(H9),
 C5(H5), C3(H3), C4(H4), C18(H18), C16(H16), C17(H17)
6.d Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C34(H34A,H34B,H34C), C33(H33A,H33B,
 H33C), C21(H21A,H21B,H21C), C25(H25A,H25B,H25C), C22(H22A,H22B,H22C), C24(H24A,
 H24B,H24C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_original_sample_id 'DIPP PHENYL'
_olex2_submission_special_instructions 'No special instructions were received'