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_7036126
_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         'C52 H50 F10 N2 O2 Rh2'
_chemical_formula_sum            'C52 H50 F10 N3 O4 Rh2'
_chemical_formula_weight         1176.77
_chemical_name_systematic
'bicyclo[2.2.1]hepta-2,5-diene{N-2,6-diisopropylphenyl(pentafluorophenyl)amidato}rhodium(I) dimer'
_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   difmap
_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                 101.855(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.4133(19)
_cell_length_b                   13.6493(13)
_cell_length_c                   20.839(2)
_cell_measurement_reflns_used    9860
_cell_measurement_temperature    90.0
_cell_measurement_theta_max      30.140
_cell_measurement_theta_min      2.228
_cell_volume                     5125.7(9)
_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 0.999
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker Apex Duo II'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0835
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.989
_diffrn_reflns_number            14974
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.140
_diffrn_reflns_theta_min         1.795
_exptl_absorpt_coefficient_mu    0.727
_exptl_absorpt_correction_T_max  0.9367
_exptl_absorpt_correction_T_min  0.8057
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0712 before and 0.0625 after correction.
The Ratio of minimum to maximum transmission is 0.8602.
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    1.525
_exptl_crystal_description       prism
_exptl_crystal_F_000             2380
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.606
_refine_diff_density_min         -0.568
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.961
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     613
_refine_ls_number_reflns         14974
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.961
_refine_ls_R_factor_all          0.0780
_refine_ls_R_factor_gt           0.0449
_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^)+(0.0352P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0824
_refine_ls_wR_factor_ref         0.0908
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10160
_reflns_number_total             14974
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt01981h2.cif
_cod_data_source_block           ls553
_cod_depositor_comments
'Adding full bibliography for 7036126--7036129.cif.'
_cod_database_code               7036126
_shelx_estimated_absorpt_t_max   0.937
_shelx_estimated_absorpt_t_min   0.806
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H10(0.029) H11(0.034) H12(0.026) H14(0.022) H15A(0.044)
 H15B(0.044) H15C(0.044) H16A(0.039) H16B(0.039) H16C(0.039) H17(0.025)
 H18A(0.041) H18B(0.041) H18C(0.041) H19A(0.046) H19B(0.046) H19C(0.046)
 H20(0.025) H21(0.03) H22(0.039) H23(0.028) H24(0.029) H25(0.034) H26A(0.052)
 H26B(0.052) H36(0.02) H37(0.019) H38(0.018) H40(0.019) H41A(0.031) H41B(0.031)
 H41C(0.031) H42A(0.036) H42B(0.036) H42C(0.036) H43(0.022) H44A(0.038)
 H44B(0.038) H44C(0.038) H45A(0.037) H45B(0.037) H45C(0.037) H46(0.024)
 H47(0.026) H48(0.029) H49(0.024) H50(0.02) H51(0.025) H52A(0.034) H52B(0.034)
 Fixed X: H10(0.6725) H11(0.5514) H12(0.5034) H14(0.5935) H15A(0.510301)
 H15B(0.5674) H15C(0.4882) H16A(0.4521) H16B(0.5085) H16C(0.476299) H17(0.8058)
 H18A(0.8106) H18B(0.869801) H18C(0.7976) H19A(0.7528) H19B(0.83) H19C(0.7568)
 H20(0.7757) H21(0.7978) H22(0.6734) H23(0.629901) H24(0.608801) H25(0.639)
 H26A(0.657901) H26B(0.5828) H36(1.0435) H37(1.081301) H38(1.0225) H40(0.8835)
 H41A(1.0008) H41B(0.9415) H41C(0.9985) H42A(0.8942) H42B(0.837) H42C(0.8305)
 H43(0.9098) H44A(0.8544) H44B(0.8797) H44C(0.9272) H45A(1.0358) H45B(0.9921)
 H45C(1.0409) H46(0.698801) H47(0.6308) H48(0.608101) H49(0.7477) H50(0.8147)
 H51(0.7174) H52A(0.591101) H52B(0.643801)
 Fixed Y: H10(0.7893) H11(0.7901) H12(0.653901) H14(0.4251) H15A(0.438999)
 H15B(0.5249) H15C(0.5453) H16A(0.488999) H16B(0.439399) H16C(0.3799)
 H17(0.602301) H18A(0.7642) H18B(0.7463) H18C(0.806) H19A(0.700399)
 H19B(0.648101) H19C(0.5862) H20(0.2551) H21(0.427) H22(0.492) H23(0.504)
 H24(0.3339) H25(0.213201) H26A(0.3124) H26B(0.3477) H36(0.0165) H37(0.0076)
 H38(0.100801) H40(0.2817) H41A(0.3275) H41B(0.3246) H41C(0.2386)
 H42A(0.119801) H42B(0.2057) H42C(0.131901) H43(0.1798) H44A(0.025301)
 H44B(0.0321) H44C(-0.027401) H45A(0.069201) H45B(0.143201) H45C(0.182)
 H46(0.2002) H47(0.27) H48(0.1302) H49(0.1349) H50(0.0654) H51(0.0167)
 H52A(0.0322) H52B(-0.0283)
 Fixed Z: H10(0.2829) H11(0.225) H12(0.166101) H14(0.1574) H15A(0.058101)
 H15B(0.061601) H15C(0.0751) H16A(0.1729) H16B(0.2303) H16C(0.1664)
 H17(0.286099) H18A(0.2414) H18B(0.306) H18C(0.308201) H19A(0.3867)
 H19B(0.396399) H19C(0.3804) H20(0.389) H21(0.434699) H22(0.4562) H23(0.3309)
 H24(0.285999) H25(0.3809) H26A(0.486199) H26B(0.439499) H36(0.3524) H37(0.254)
 H38(0.1664) H40(0.168401) H41A(0.149) H41B(0.0832) H41C(0.101001) H42A(0.0858)
 H42B(0.068701) H42C(0.124901) H43(0.3947) H44A(0.365001) H44B(0.4414)
 H44C(0.400599) H45A(0.4552) H45B(0.4907) H45C(0.442599) H46(0.117001)
 H47(0.199901) H48(0.2751) H49(0.3248) H50(0.2408) H51(0.1394) H52A(0.1696)
 H52B(0.226)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'