Isocyanate deinsertion from κ(1)-O amidates: facile access to perfluoroaryl rhodium(i) complexes.
Drover, Marcus W.; Schafer, Laurel L.; Love, Jennifer A.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 19487–19493; doi:10.1039/c5dt01981h

data_7036128
_publ_section_title
;
 Isocyanate deinsertion from \k(1)-O amidates: facile access to
 perfluoroaryl rhodium(i) complexes.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              19487
_journal_page_last               19493
_journal_paper_doi               10.1039/c5dt01981h
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C60 H45 F5 P3 Rh, 0.99(C6 H14)'
_chemical_formula_sum            'C65.94 H58.86 F5 P3 Rh'
_chemical_formula_weight         1142.12
_chemical_name_systematic
tris(triphenylphosphine)(pentafluorophenyl)rhodium(I)
_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     direct
_audit_creation_date             2015-05-26
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-05-26 deposited with the CCDC.
2015-08-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.3810(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1408(7)
_cell_length_b                   37.184(2)
_cell_length_c                   12.9377(8)
_cell_measurement_reflns_used    9989
_cell_measurement_temperature    90.0
_cell_measurement_theta_max      26.018
_cell_measurement_theta_min      2.290
_cell_volume                     5326.4(6)
_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, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      90.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Apex Duo II'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0827
_diffrn_reflns_av_unetI/netI     0.0669
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            49268
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.062
_diffrn_reflns_theta_min         1.919
_exptl_absorpt_coefficient_mu    0.471
_exptl_absorpt_correction_T_max  0.9547
_exptl_absorpt_correction_T_min  0.4922
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0675 before and 0.0611 after correction.
The Ratio of minimum to maximum transmission is 0.9369.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_description       plate
_exptl_crystal_F_000             2358
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.739
_refine_diff_density_min         -0.449
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     733
_refine_ls_number_reflns         10500
_refine_ls_number_restraints     711
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.0694
_refine_ls_R_factor_gt           0.0414
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0261P)^2^+5.3951P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0765
_refine_ls_wR_factor_ref         0.0853
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7778
_reflns_number_total             10500
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt01981h2.cif
_cod_data_source_block           mo_ls579_0m_a
_cod_depositor_comments
'Adding full bibliography for 7036126--7036129.cif.'
_cod_database_code               7036128
_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
 C61-C62
 1.54 with sigma of 0.01
 C68-C67
 1.54 with sigma of 0.01
 C75-C74 = C74-C73
 1.54 with sigma of 0.01
 C78-C77
 1.54 with sigma of 0.01
 C62-C61 \\sim C63-C62 \\sim C64-C63 \\sim C65-C64 \\sim C66-C65
 with sigma of 0.01
 C61-C63 \\sim C62-C64 \\sim C63-C65 \\sim C64-C66
 with sigma of 0.01
 C68-C67 \\sim C69-C68 \\sim C70-C69 \\sim C71-C70 \\sim C72-C71
 with sigma of 0.01
 C67-C69 \\sim C68-C70 \\sim C69-C71 \\sim C70-C72
 with sigma of 0.01
 C74-C73 \\sim C75-C74 \\sim C76-C75 \\sim C77-C76 \\sim C78-C77
 with sigma of 0.01
 C73-C75 \\sim C74-C76 \\sim C75-C77 \\sim C76-C78
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C72) = Uanis(C66) = Uanis(C78)
Uanis(C65) = Uanis(C71) = Uanis(C77)
Uanis(C64) = Uanis(C76)
Uanis(C70) = Uanis(C75) = Uanis(C63)
Uanis(C74) = Uanis(C67)
Uanis(C73) = Uanis(C68) = Uanis(C62)
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 1*[Sof(C62)+Sof(H62A)+Sof(H62B)+Sof(C65)+Sof(H65A)+Sof(H65B)+Sof(C66)+
 Sof(H66A)+Sof(H66B)+Sof(H66C)+Sof(C63)+Sof(H63A)+Sof(H63B)+Sof(C64)+Sof(H64A)+
 Sof(H64B)+Sof(C61)+Sof(H61A)+Sof(H61B)+Sof(H61C)]+1*[Sof(C70)+Sof(H70A)+
 Sof(H70B)+Sof(C68)+Sof(H68A)+Sof(H68B)+Sof(C69)+Sof(H69A)+Sof(H69B)+Sof(C72)+
 Sof(H72A)+Sof(H72B)+Sof(H72C)+Sof(C71)+Sof(H71A)+Sof(H71B)+Sof(C67)+Sof(H67A)+
 Sof(H67B)+Sof(H67C)]+1*[Sof(C73)+Sof(H73A)+Sof(H73B)+Sof(H73C)+Sof(C74)+
 Sof(H74A)+Sof(H74B)+Sof(C75)+Sof(H75A)+Sof(H75B)+Sof(C76)+Sof(H76A)+Sof(H76B)+
 Sof(C77)+Sof(H77A)+Sof(H77B)+Sof(C78)+Sof(H78A)+Sof(H78B)+Sof(H78C)]=1 with
 esd of 0.003
 Sof(C62)=Sof(H62A)=Sof(H62B)=Sof(C65)=Sof(H65A)=Sof(H65B)=Sof(C66)=Sof(H66A)=
 Sof(H66B)=Sof(H66C)=Sof(C63)=Sof(H63A)=Sof(H63B)=Sof(C64)=Sof(H64A)=Sof(H64B)=
 Sof(C61)=Sof(H61A)=Sof(H61B)=Sof(H61C)=FVAR(1)
 Sof(C70)=Sof(H70A)=Sof(H70B)=Sof(C68)=Sof(H68A)=Sof(H68B)=Sof(C69)=Sof(H69A)=
 Sof(H69B)=Sof(C72)=Sof(H72A)=Sof(H72B)=Sof(H72C)=Sof(C71)=Sof(H71A)=Sof(H71B)=
 Sof(C67)=Sof(H67A)=Sof(H67B)=Sof(H67C)=FVAR(2)
 Sof(C73)=Sof(H73A)=Sof(H73B)=Sof(H73C)=Sof(C74)=Sof(H74A)=Sof(H74B)=Sof(C75)=
 Sof(H75A)=Sof(H75B)=Sof(C76)=Sof(H76A)=Sof(H76B)=Sof(C77)=Sof(H77A)=Sof(H77B)=
 Sof(C78)=Sof(H78A)=Sof(H78B)=Sof(H78C)=FVAR(3)
6.a Secondary CH2 refined with riding coordinates:
 C62(H62A,H62B), C65(H65A,H65B), C63(H63A,H63B), C64(H64A,H64B), C70(H70A,
 H70B), C68(H68A,H68B), C69(H69A,H69B), C71(H71A,H71B), C74(H74A,H74B),
 C75(H75A,H75B), C76(H76A,H76B), C77(H77A,H77B)
6.b Aromatic/amide H refined with riding coordinates:
 C27(H27), C50(H50), C12(H12), C28(H28), C39(H39), C6(H6), C2(H2), C37(H37),
 C8(H8), C3(H3), C16(H16), C43(H43), C51(H51), C47(H47), C18(H18), C11(H11),
 C52(H52), C31(H31), C46(H46), C45(H45), C40(H40), C41(H41), C20(H20), C44(H44),
  C33(H33), C14(H14), C24(H24), C25(H25), C29(H29), C23(H23), C21(H21),
 C22(H22), C15(H15), C30(H30), C34(H34), C35(H35), C36(H36), C54(H54), C9(H9),
 C53(H53), C5(H5), C10(H10), C4(H4), C42(H42), C13(H13)
6.c Idealised Me refined as rotating group:
 C66(H66A,H66B,H66C), C61(H61A,H61B,H61C), C72(H72A,H72B,H72C), C67(H67A,H67B,
 H67C), C73(H73A,H73B,H73C), C78(H78A,H78B,H78C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'