Rhodium(I) Complexes of the Conformationally Rigid IBioxMe4 Ligand: Preparation of Mono-, Bis-, and Tris-ligated NHC Complexes
Chaplin, Adrian B.; Organometallics 33 (2014) 3069–; doi:10.1021/om500332n

data_4089665
_publ_section_title
;
 Rhodium(I) Complexes of the Conformationally Rigid IBioxMe4 Ligand:
 Preparation of Mono-, Bis-, and Tris-ligated NHC Complexes
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              3069
_journal_paper_doi               10.1021/om500332n
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C29 H40 N4 O4 Rh, C32 H12 B F24'
_chemical_formula_sum            'C61 H52 B F24 N4 O4 Rh'
_chemical_formula_weight         1474.78
_chemical_melting_point          ?
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-10-27
_audit_creation_method
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.4704(10)
_cell_length_b                   22.8734(5)
_cell_length_c                   16.2804(4)
_cell_measurement_reflns_used    25367
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.5624
_cell_measurement_theta_min      2.7858
_cell_volume                     6133.4(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_molecular_graphics
;
Ortep-3 for Windows: L. J. Farrugia, J. Appl. Cryst (1997), 30, 565.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.2833
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -38.00   87.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       22.0171  -19.0000   60.0000 125

  2 omega  -77.00  -39.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.9546  125.0000   27.0000 38

  3 omega  -15.00  106.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       22.0171   57.0000  120.0000 121

  4 omega  -15.00  106.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       22.0171   57.0000 -120.0000 121

  5 omega   61.00  107.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       22.0171  146.0000   13.0000 46

  6 omega -119.00  -57.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.9546 -178.0000 -150.0000 62
;
_diffrn_measurement_device_type  'Oxford Diffraction: Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0420839000
_diffrn_orient_matrix_UB_12      -0.0056389000
_diffrn_orient_matrix_UB_13      -0.0047681000
_diffrn_orient_matrix_UB_21      0.0085093000
_diffrn_orient_matrix_UB_22      0.0299809000
_diffrn_orient_matrix_UB_23      0.0068897000
_diffrn_orient_matrix_UB_31      0.0033190000
_diffrn_orient_matrix_UB_32      -0.0054652000
_diffrn_orient_matrix_UB_33      0.0427510000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_unetI/netI     0.0193
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            73654
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        29.575
_diffrn_reflns_theta_max         29.575
_diffrn_reflns_theta_min         2.911
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.403
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98067
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.597
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2976
_exptl_crystal_recrystallization_method
'Crystals grown from C6H4F2-Heptane at 293 K'
_exptl_crystal_size_max          0.5000
_exptl_crystal_size_mid          0.1800
_exptl_crystal_size_min          0.1500
_refine_diff_density_max         0.645
_refine_diff_density_min         -0.559
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     490
_refine_ls_number_reflns         8596
_refine_ls_number_restraints     252
_refine_ls_restrained_S_all      1.296
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0382
_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^)+(0.0312P)^2^+6.2410P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0838
_refine_ls_wR_factor_ref         0.0876
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7467
_reflns_number_total             8596
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500332n_si_002.cif
_cod_data_source_block           10
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value 'not measured' was changed
to '?' -- the value is undefined or not given.

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               4089665
_shelxl_version_number           2013-4
_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
 C207-F1 \\sim C207-F2 \\sim C207-F3 \\sim C207-F101 \\sim C207-F102 \\sim
C207-F103
 with sigma of 0.01
 F1-F2 \\sim F2-F3 \\sim F3-F1 \\sim F101-F102 \\sim F102-F103 \\sim F103-F101
 with sigma of 0.01
 C203-F1 \\sim C203-F2 \\sim C203-F3 \\sim C203-F101 \\sim C203-F102 \\sim
C203-F103
 with sigma of 0.01
 C215-F7 \\sim C215-F8 \\sim C215-F9 \\sim C215-F107 \\sim C215-F108 \\sim
C215-F109
 with sigma of 0.01
 F7-F8 \\sim F8-F9 \\sim F9-F7 \\sim F107-F108 \\sim F108-F109 \\sim F109-F107
 with sigma of 0.01
 C211-F7 \\sim C211-F8 \\sim C211-F9 \\sim C211-F107 \\sim C211-F108 \\sim
C211-F109
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
F1 \\sim F2 \\sim F3 \\sim F4 \\sim F5 \\sim F6 \\sim F7 \\sim F8 \\sim F9
\\sim F10 \\sim F11 \\sim F12 \\sim F101 \\sim F102 \\sim F103 \\sim F107 \\sim
F108 \\sim F109: within 1.7A with sigma of 0.007 and sigma for terminal atoms
of 0.01
Uanis(F1) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F4) \\sim
Ueq, Uanis(F5) \\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F7) \\sim Ueq, Uanis(F8)
\\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(F10) \\sim Ueq, Uanis(F11) \\sim Ueq,
Uanis(F12) \\sim Ueq, Uanis(F101) \\sim Ueq, Uanis(F102) \\sim Ueq, Uanis(F103)
\\sim Ueq, Uanis(F107) \\sim Ueq, Uanis(F108) \\sim Ueq, Uanis(F109) \\sim Ueq:
with sigma of 0.007 and sigma for terminal atoms of 0.01
4. Others
 Sof(F107)=Sof(F108)=Sof(F109)=1-FVAR(1)
 Sof(F7)=Sof(F8)=Sof(F9)=FVAR(1)
 Sof(F101)=Sof(F102)=Sof(F103)=1-FVAR(2)
 Sof(F1)=Sof(F2)=Sof(F3)=FVAR(2)
 Fixed Sof: H5A(0.5) H5B(0.5)
5.a Ternary CH refined with riding coordinates:
 C2(H2), C3(H3), C4(H4)
5.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C12(H12A,H12B), C15(H15A,H15B)
5.c Aromatic/amide H refined with riding coordinates:
 C202(H202), C204(H204), C206(H206), C210(H210), C212(H212), C214(H214)
5.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C)
;