Methanol as hydrogen source: transfer hydrogenation of aromatic aldehydes with a rhodacycle.
Aboo, Ahmed H.; Bennett, Elliot L.; Deeprose, Mark; Robertson, Craig M.; Iggo, Jonathan A.; Xiao, Jianliang; Chemical communications (Cambridge, England) 54 (2018) 11805–11808; doi:10.1039/c8cc06612d

data_7122417
_publ_section_title
;
 Methanol as hydrogen source: transfer hydrogenation of aromatic aldehydes
 with a rhodacycle.
;
_journal_issue                   83
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              11805
_journal_page_last               11808
_journal_paper_doi               10.1039/c8cc06612d
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C25 H29 Cl N O2 Rh'
_chemical_formula_sum            'C25 H29 Cl N O2 Rh'
_chemical_formula_weight         513.85
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-04-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.03 svn.r3497 for OlexSys, GUI svn.r5486)
;
_audit_update_record
;
2018-06-25 deposited with the CCDC.
2018-09-25 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 103.076(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.6375(3)
_cell_length_b                   13.8673(4)
_cell_length_c                   18.4717(6)
_cell_measurement_reflns_used    11820
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.3840
_cell_measurement_theta_min      1.8570
_cell_volume                     2155.15(12)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -110.00  15.00   1.00   10.00    --  -20.00 -68.00   0.00  125
  2  \w   -110.00  15.00   1.00   10.00    --  -20.00 -68.00 120.00  125
  3  \w   -110.00  15.00   1.00   10.00    --  -20.00 -68.00 240.00  125
  4  \w   -110.00  15.00   1.00   10.00    --  -20.00 -30.00  90.00  125
  5  \w    -90.00  90.00   1.00    1.00    --    0.00   0.00   0.00  180
;
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  Rigaku_AFC12K_724P_007HF_Mo
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'Mitegen 10um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0394053000
_diffrn_orient_matrix_UB_12      -0.0206940000
_diffrn_orient_matrix_UB_13      0.0260251000
_diffrn_orient_matrix_UB_21      -0.0102907000
_diffrn_orient_matrix_UB_22      0.0465537000
_diffrn_orient_matrix_UB_23      0.0140898000
_diffrn_orient_matrix_UB_31      -0.0738176000
_diffrn_orient_matrix_UB_32      0.0045442000
_diffrn_orient_matrix_UB_33      -0.0260419000
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.710747
_diffrn_reflns_av_R_equivalents  0.1371
_diffrn_reflns_av_unetI/netI     0.0711
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            34723
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.85
_diffrn_source                   'Rotating Anode'
_diffrn_source_type              'Rotating Anode'
_exptl_absorpt_coefficient_mu    0.939
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94934
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.584
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.005
_refine_diff_density_max         0.594
_refine_diff_density_min         -0.617
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     279
_refine_ls_number_reflns         4406
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0477
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0148P)^2^+4.7449P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0794
_refine_ls_wR_factor_ref         0.0868
_reflns_number_gt                3499
_reflns_number_total             4406
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8cc06612d2.cif
_cod_data_source_block           eb_c1
_cod_depositor_comments          'Adding full bibliography for 7122417.cif.'
_cod_database_code               7122417
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.31
_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, All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C10(H10), C13(H13), C7(H7), C11(H11), C14(H14)
2.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C24(H24A,H24B,H24C), C15(H15A,H15B,H15C), C25(H25A,H25B,
 H25C), C22(H22A,H22B,H22C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C)
2.c Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.157
_oxdiff_exptl_absorpt_empirical_full_min 0.897