C2-Selective silylation of pyridines by a rhodium-aluminum complex.
Hara, Naofumi; Uemura, Nao; Nakao, Yoshiaki; Chemical communications (Cambridge, England) 57 (2021) 5957–5960; doi:10.1039/d1cc00278c

data_7128278
_publ_section_title
;
 C2-Selective silylation of pyridines by a rhodium-aluminum complex.
;
_journal_issue                   48
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              5957
_journal_page_last               5960
_journal_paper_doi               10.1039/d1cc00278c
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C53 H53 Al N5 P2 Rh'
_chemical_formula_sum            'C53 H53 Al N5 P2 Rh'
_chemical_formula_weight         951.83
_chemical_name_systematic
(\h2,\h2-bicyclo[2.2.1]hepta-2,5-diene)-(N,N-bis(2-(diphenylphosphinomethylamido)phenyl)methylamine)-(4-dimethylaminopyridine)-aluminium-rhodium
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_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
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Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
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_audit_update_record
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2021-01-15 deposited with the CCDC.	2021-05-04 downloaded from the CCDC.
;
_cell_angle_alpha                90.03(5)
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_cell_length_b                   11.89(3)
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_computing_cell_refinement
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CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
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_computing_data_collection
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CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
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_computing_data_reduction
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CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
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_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
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_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      143.15
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_details
;
scan:
	Number of images: 360
	           Slice: -110.0000 - 70.0000
	     Image width: 0.5000
	        Exp time: 8.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 0.0000
	             XTD: 44.9714
	          2theta: -20.0248
scan:
	Number of images: 360
	           Slice: -110.0000 - 70.0000
	     Image width: 0.5000
	        Exp time: 8.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 90.0000
	             XTD: 44.9714
	          2theta: -20.0248
;
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_unetI/netI     0.0683
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.953
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_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19679
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.492
_diffrn_reflns_theta_min         3.030
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.479
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.812
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_description       block
_exptl_crystal_F_000             988
_exptl_crystal_preparation       Loop
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene/hexane'
_exptl_crystal_size_max          0.12
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_refine_diff_density_min         -0.707
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     562
_refine_ls_number_reflns         10587
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0464
_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^)+(0.0327P)^2^+0.7459P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0915
_refine_ls_wR_factor_ref         0.0969
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_reflns_number_gt                9094
_reflns_number_total             10587
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc00278c2.cif
_cod_data_source_block           '_15_14_002b'
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7128277--7128278.cif.
;
_cod_database_code               7128278
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.958
_shelx_estimated_absorpt_t_min   0.945
_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.a Ternary CH refined with riding coordinates:
 C40(H40), C41(H41), C45(H45), C44(H44), C42(H42), C43(H43)
2.b Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C13(H13A,H13B), C46(H46A,H46B)
2.c Aromatic/amide H refined with riding coordinates:
 C51(H51), C47(H47), C50(H50), C12(H12), C18(H18), C39(H39), C48(H48),
 C35(H35), C22(H22), C33(H33), C29(H29), C23(H23), C8(H8), C38(H38), C15(H15),
 C16(H16), C25(H25), C24(H24), C37(H37), C11(H11), C32(H32), C6(H6), C36(H36),
 C30(H30), C10(H10), C2(H2), C31(H31), C17(H17), C3(H3), C9(H9), C5(H5), C4(H4)
2.d Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C)
;
_smtbx_masks_void_probe_radius   1.2
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_olex2_submission_special_instructions 'No special instructions were received'