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_7036127
_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         'C44 H58 F5 N O P Rh, 0.25(C6 H14)'
_chemical_formula_sum            'C45.5 H61.5 F5 N O P Rh'
_chemical_formula_weight         867.33
_chemical_name_systematic
'bicyclo[2.2.1]hepta-2,5-diene{N-2,6-diisopropylphenyl(pentafluorophenyl)amidato}tricyclohexylphosphine rhodium(I)'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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                102.878(3)
_cell_angle_beta                 99.532(3)
_cell_angle_gamma                90.372(3)
_cell_formula_units_Z            4
_cell_length_a                   9.9058(8)
_cell_length_b                   21.0289(17)
_cell_length_c                   21.6355(16)
_cell_measurement_temperature    90
_cell_volume                     4328.4(6)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      90
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker Apex-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0779
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            15659
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.401
_diffrn_reflns_theta_max         25.401
_diffrn_reflns_theta_min         1.227
_exptl_absorpt_coefficient_mu    0.487
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0813 before and 0.0672 after correction.
 The Ratio of minimum to maximum transmission is 0.77.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 155808 reflections, Rint = 0.1134
 (42370 with I > 3sig(I), Rint = 0.0704)
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_description       cube
_exptl_crystal_F_000             1818
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.140
_refine_diff_density_min         -1.210
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     991
_refine_ls_number_reflns         15659
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0798
_refine_ls_R_factor_gt           0.0528
_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^)+(0.0798P)^2^+1.5366P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1349
_refine_ls_wR_factor_ref         0.1457
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11473
_reflns_number_total             15659
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt01981h2.cif
_cod_data_source_block           ls591t4_a_sq_s
_cod_depositor_comments
'Adding full bibliography for 7036126--7036129.cif.'
_cod_original_formula_sum        'C45.50 H61.50 F5 N O P Rh'
_cod_database_code               7036127
_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:
 C66(H66), C71(H71), C72(H72), C84(H84), C68(H68), C65(H65), C78(H78),
 C59(H59), C67(H67), C70(H70), C20(H20), C17(H17), C25(H25), C62(H62), C14(H14),
  C39(H39), C40(H40), C23(H23), C21(H21), C26(H26), C27(H27), C22(H22)
2.b Secondary CH2 refined with riding coordinates:
 C89(H89A,H89B), C85(H85A,H85B), C87(H87A,H87B), C83(H83A,H83B), C88(H88A,
 H88B), C73(H73A,H73B), C79(H79A,H79B), C38(H38A,H38B), C37(H37A,H37B),
 C34(H34A,H34B), C32(H32A,H32B), C80(H80A,H80B), C76(H76A,H76B), C82(H82A,H82B),
  C45(H45A,H45B), C69(H69A,H69B), C86(H86A,H86B), C77(H77A,H77B), C75(H75A,
 H75B), C74(H74A,H74B), C81(H81A,H81B), C36(H36A,H36B), C41(H41A,H41B),
 C42(H42A,H42B), C43(H43A,H43B), C30(H30A,H30B), C31(H31A,H31B), C28(H28A,H28B),
  C24(H24A,H24B), C44(H44A,H44B), C35(H35A,H35B), C29(H29A,H29B), C02Z(H02A,
 H02B), C030(H03A,H03B)
2.c Aromatic/amide H refined with riding coordinates:
 C57(H57), C55(H55), C12(H12), C56(H56), C10(H10), C11(H11)
2.d Idealised Me refined as rotating group:
 C61(H61A,H61B,H61C), C60(H60A,H60B,H60C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C19(H19A,H19B,H19C), C64(H64A,H64B,H64C), C63(H63A,H63B,H63C), C18(H18A,
 H18B,H18C), C031(H03C,H03D,H03E)
;
_shelx_fab_checksum              12033
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'