(Diphenylphosphino)alkylaldehyde affords hydride- or alkyl-[(diphenylphosphino)alkylacyl]rhodium(iii) or (diphenylphosphino)alkylester complexes: theoretical and experimental diastereoselectivity.
Azpeitia, Susan; Barquín, Montserrat; Mendicute-Fierro, Claudio; Huertos, Miguel A.; Rodríguez-Diéguez, Antonio; Seco, Jose M.; San Sebastian, Eider; Ibarlucea, Lourdes; Garralda, María A; Dalton transactions (Cambridge, England : 2003) 48 (2019) 3300–3313; doi:10.1039/c8dt04929g

data_7048852
_publ_section_title
;
 (Diphenylphosphino)alkylaldehyde affords hydride- or
 alkyl-[(diphenylphosphino)alkylacyl]rhodium(iii) or
 (diphenylphosphino)alkylester complexes: theoretical and experimental
 diastereoselectivity.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3300
_journal_page_last               3313
_journal_paper_doi               10.1039/c8dt04929g
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C49 H40 N2 O P2 Rh, B F4'
_chemical_formula_sum            'C57 H60 B F4 N2 O3 P2 Rh'
_chemical_formula_weight         1072.73
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-02-08
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2018-12-13 deposited with the CCDC.
2019-02-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.271(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.685(3)
_cell_length_b                   29.093(3)
_cell_length_c                   20.488(4)
_cell_measurement_reflns_used    6485
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      14.963
_cell_measurement_theta_min      2.356
_cell_volume                     5935(2)
_computing_cell_refinement       'Bruker ApexII'
_computing_data_collection       'Bruker ApexII'
_computing_data_reduction        'Bruker ApexII'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'Phi and Omega Scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_unetI/netI     0.0218
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            15647
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        14.973
_diffrn_reflns_theta_max         14.973
_diffrn_reflns_theta_min         2.162
_exptl_absorpt_coefficient_mu    0.394
_exptl_absorpt_correction_T_max  0.7439
_exptl_absorpt_correction_T_min  0.6143
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0936 before and 0.0475 after correction.
The Ratio of minimum to maximum transmission is 0.8258.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.201
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2224
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.695
_refine_diff_density_min         -0.461
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.190
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         2378
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.190
_refine_ls_R_factor_all          0.0810
_refine_ls_R_factor_gt           0.0770
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0371P)^2^+133.4457P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1788
_refine_ls_wR_factor_ref         0.1812
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2214
_reflns_number_total             2378
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04929g2.cif
_cod_data_source_block           Compound7a
_cod_depositor_comments
'Adding full bibliography for 7048850--7048854.cif.'
_cod_database_code               7048852
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C1-H
 2.4 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C22(H22)
3.b Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C24(H24),
  C25(H25), C26(H26), C27(H27), C28(H28), C30(H30), C31(H31), C32(H32),
 C33(H33), C34(H34), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C42(H42),
  C43(H43), C44(H44), C47(H47), C48(H48), C49(H49)
;
_shelx_res_checksum              73586
_shelx_fab_checksum              13850
_olex2_submission_special_instructions 'No special instructions were received'