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_7036129
_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         'C31 H41 F5 P Rh'
_chemical_formula_sum            'C31 H41 F5 P Rh'
_chemical_formula_weight         642.52
_chemical_name_systematic
bicyclo[2.2.1]hepta-2,5-dienetricyclohexylphosphinepentafluorophenylrhodium
_chemical_properties_physical    'Air-sensitive, Hygroscopic'
_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             2015-07-17
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-07-19 deposited with the CCDC.
2015-08-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.257(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.6503(12)
_cell_length_b                   20.980(2)
_cell_length_c                   11.7247(13)
_cell_measurement_temperature    90
_cell_volume                     2865.1(5)
_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
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker Apex Duo II'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_unetI/netI     0.0247
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            35522
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.559
_diffrn_reflns_theta_min         1.941
_exptl_absorpt_coefficient_mu    0.704
_exptl_absorpt_correction_T_max  0.9519
_exptl_absorpt_correction_T_min  0.7842
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0554 before and 0.0422 after correction.
The Ratio of minimum to maximum transmission is 0.8238.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_description       prism
_exptl_crystal_F_000             1328
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: hexanes'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.689
_refine_diff_density_min         -0.960
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         8756
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0355
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0383P)^2^+5.4799P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0891
_refine_ls_wR_factor_ref         0.0927
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7918
_reflns_number_total             8756
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt01981h2.cif
_cod_data_source_block           mo_jl148_0m_a
_cod_depositor_comments
'Adding full bibliography for 7036126--7036129.cif.'
_cod_original_cell_volume        2865.2(5)
_cod_database_code               7036129
_shelx_estimated_absorpt_t_max   0.952
_shelx_estimated_absorpt_t_min   0.766
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C14(H14), C20(H20), C26(H26), C10(H10), C11(H11), C8(H8), C9(H9), C12(H12),
 C7(H7)
2.b Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C25(H25A,H25B), C19(H19A,H19B), C15(H15A,H15B), C27(H27A,
 H27B), C16(H16A,H16B), C22(H22A,H22B), C31(H31A,H31B), C24(H24A,H24B),
 C17(H17A,H17B), C30(H30A,H30B), C23(H23A,H23B), C18(H18A,H18B), C29(H29A,H29B),
  C28(H28A,H28B), C13(H13A,H13B)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'