Rhodium(I) Complexes of the Conformationally Rigid IBioxMe4 Ligand: Isolation of a Stable Low-Coordinate T-Shaped Complex
Chaplin, Adrian B.; Organometallics 33 (2014) 624–; doi:10.1021/om401223w

data_4089654
_publ_section_title
;
 Rhodium(I) Complexes of the Conformationally Rigid IBioxMe4 Ligand:
 Isolation of a Stable Low-Coordinate T-Shaped Complex
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              624
_journal_paper_doi               10.1021/om401223w
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C34 H47 N6 O7 Rh, C32 H12 B F24'
_chemical_formula_sum            'C66 H59 B F24 N6 O7 Rh'
_chemical_formula_weight         1617.91
_chemical_melting_point          ?
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-10-28
_audit_creation_method
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_cell_angle_alpha                105.287(3)
_cell_angle_beta                 101.319(3)
_cell_angle_gamma                93.354(2)
_cell_formula_units_Z            2
_cell_length_a                   13.1514(4)
_cell_length_b                   13.4750(4)
_cell_length_c                   21.9169(7)
_cell_measurement_reflns_used    8107
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.6920
_cell_measurement_theta_min      3.0242
_cell_volume                     3648.7(2)
_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
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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 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Oxford Diffraction: Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0263439000
_diffrn_orient_matrix_UB_12      -0.0339686000
_diffrn_orient_matrix_UB_13      -0.0303820000
_diffrn_orient_matrix_UB_21      0.0069012000
_diffrn_orient_matrix_UB_22      0.0397448000
_diffrn_orient_matrix_UB_23      -0.0150512000
_diffrn_orient_matrix_UB_31      0.0482224000
_diffrn_orient_matrix_UB_32      -0.0168900000
_diffrn_orient_matrix_UB_33      -0.0057607000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_unetI/netI     0.0765
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            23624
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         3.030
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.349
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84753
_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            'pale yellow'
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1638
_exptl_crystal_recrystallization_method
'Crystals grown from C6H4F2-Heptane at 293 K'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.817
_refine_diff_density_min         -0.567
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1190
_refine_ls_number_reflns         12825
_refine_ls_number_restraints     1320
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0854
_refine_ls_R_factor_gt           0.0639
_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^)+(0.0742P)^2^+1.2796P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1430
_refine_ls_wR_factor_ref         0.1537
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10161
_reflns_number_total             12825
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om401223w_si_002.cif
_cod_data_source_block           0026abc13
_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               4089654
_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
 C215-F7 \\sim C215-F8 \\sim C215-F9 \\sim C315-F107 \\sim C315-F108 \\sim
C315-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
 C211-C215 \\sim C211-C315
 with sigma of 0.01
 C216-F10 \\sim C216-F11 \\sim C216-F12 \\sim C316-F110 \\sim C316-F111 \\sim
C316-F112
 with sigma of 0.01
 F10-F11 \\sim F11-F12 \\sim F12-F10 \\sim F110-F111 \\sim F111-F112 \\sim
F112-F110
 with sigma of 0.01
 C213-F10 \\sim C213-F11 \\sim C213-F12 \\sim C213-F110 \\sim C213-F111 \\sim
C213-F112
 with sigma of 0.01
 C213-C216 \\sim C213-C316
 with sigma of 0.01
 C224-F16 \\sim C224-F17 \\sim C224-F18 \\sim C324-F116 \\sim C324-F117 \\sim
C324-F118
 with sigma of 0.01
 F16-F17 \\sim F17-F18 \\sim F18-F16 \\sim F116-F117 \\sim F117-F118 \\sim
F118-F116
 with sigma of 0.01
 C221-F16 \\sim C221-F17 \\sim C221-F18 \\sim C221-F116 \\sim C221-F117 \\sim
C221-F118
 with sigma of 0.01
 C221-C224 \\sim C221-C324
 with sigma of 0.01
 C231-F19 \\sim C231-F20 \\sim C231-F21 \\sim C331-F119 \\sim C331-F120 \\sim
C331-F121
 with sigma of 0.01
 F19-F20 \\sim F20-F21 \\sim F21-F19 \\sim F119-F120 \\sim F120-F121 \\sim
F121-F119
 with sigma of 0.01
 C227-F19 \\sim C227-F20 \\sim C227-F21 \\sim C227-F119 \\sim C227-F120 \\sim
C227-F121
 with sigma of 0.01
 C227-C231 \\sim C227-C331
 with sigma of 0.01
 C232-F22 \\sim C232-F23 \\sim C232-F24 \\sim C332-F122 \\sim C332-F123 \\sim
C332-F124
 with sigma of 0.01
 F22-F23 \\sim F23-F24 \\sim F24-F22 \\sim F122-F123 \\sim F123-F124 \\sim
F124-F122
 with sigma of 0.01
 C229-F22 \\sim C229-F23 \\sim C229-F24 \\sim C229-F122 \\sim C229-F123 \\sim
C229-F124
 with sigma of 0.01
 C229-C232 \\sim C229-C332
 with sigma of 0.01
 C42-C47 \\sim C42-C48 \\sim C42-C147 \\sim C42-C148
 with sigma of 0.01
 C47-C48 \\sim C147-C148
 with sigma of 0.01
 C43-C47 \\sim C43-C48 \\sim C43-C147 \\sim C43-C148
 with sigma of 0.01
 O3B-C2B \\sim O3A-C2A \\sim O3-C2
 with sigma of 0.007
 Rh1-C2B \\sim Rh1-C2A \\sim Rh1-C2
 with sigma of 0.007
 Rh1-O3A \\sim Rh1-O3 \\sim Rh1-O3B
 with sigma of 0.01
 C2-C2A \\sim C2-C2B
 with sigma of 0.01
 O3-O3A \\sim O3-O3B
 with sigma of 0.01
3. Restrained planarity
 Rh1, C2A, O3A, C2, O3, C2B, O3B
 with sigma of 0.01
4. 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 F13 \\sim F14 \\sim F15 \\sim F16 \\sim F17
\\sim F18 \\sim F19 \\sim F20 \\sim F21 \\sim F22 \\sim F23 \\sim F24 \\sim
F101 \\sim F102 \\sim F103 \\sim F104 \\sim F105 \\sim F106 \\sim F107 \\sim
F108 \\sim F109 \\sim F110 \\sim F111 \\sim F112 \\sim F116 \\sim F117 \\sim
F118 \\sim F119 \\sim F120 \\sim F121 \\sim F122 \\sim F123 \\sim F124 \\sim
C324 \\sim C224 \\sim C315 \\sim C215 \\sim C316 \\sim C216 \\sim C332 \\sim
C232 \\sim C331 \\sim C231 \\sim C47 \\sim C48 \\sim C147 \\sim C148 \\sim C2A
\\sim C2 \\sim C2B \\sim O3A \\sim O3 \\sim O3B: within 1.7A with sigma of 0.01
and sigma for terminal atoms of 0.02
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(F13) \\sim Ueq, Uanis(F14) \\sim Ueq, Uanis(F15)
\\sim Ueq, Uanis(F16) \\sim Ueq, Uanis(F17) \\sim Ueq, Uanis(F18) \\sim Ueq,
Uanis(F19) \\sim Ueq, Uanis(F20) \\sim Ueq, Uanis(F21) \\sim Ueq, Uanis(F22)
\\sim Ueq, Uanis(F23) \\sim Ueq, Uanis(F24) \\sim Ueq, Uanis(F101) \\sim Ueq,
Uanis(F102) \\sim Ueq, Uanis(F103) \\sim Ueq, Uanis(F104) \\sim Ueq,
Uanis(F105) \\sim Ueq, Uanis(F106) \\sim Ueq, Uanis(F107) \\sim Ueq,
Uanis(F108) \\sim Ueq, Uanis(F109) \\sim Ueq, Uanis(F110) \\sim Ueq,
Uanis(F111) \\sim Ueq, Uanis(F112) \\sim Ueq, Uanis(F116) \\sim Ueq,
Uanis(F117) \\sim Ueq, Uanis(F118) \\sim Ueq, Uanis(F119) \\sim Ueq,
Uanis(F120) \\sim Ueq, Uanis(F121) \\sim Ueq, Uanis(F122) \\sim Ueq,
Uanis(F123) \\sim Ueq, Uanis(F124) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C324) \\sim Ueq, Uanis(C224) \\sim Ueq, Uanis(C315) \\sim Ueq,
Uanis(C215) \\sim Ueq, Uanis(C316) \\sim Ueq, Uanis(C216) \\sim Ueq,
Uanis(C332) \\sim Ueq, Uanis(C232) \\sim Ueq, Uanis(C331) \\sim Ueq,
Uanis(C231) \\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C147)
\\sim Ueq, Uanis(C148) \\sim Ueq, Uanis(C2A) \\sim Ueq, Uanis(C2) \\sim Ueq,
Uanis(C2B) \\sim Ueq, Uanis(O3A) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(O3B)
\\sim Ueq: with sigma of 0.007 and sigma for terminal atoms of 0.002
Uanis(C324) = Uanis(C224)
Uanis(C315) = Uanis(C215)
Uanis(C316) = Uanis(C216)
Uanis(C332) = Uanis(C232)
Uanis(C331) = Uanis(C231)
Uanis(C47) = Uanis(C147)
Uanis(C48) = Uanis(C148)
Uanis(C2A) = Uanis(C2) = Uanis(C2B)
Uanis(O3A) = Uanis(O3) = Uanis(O3B)
5. Others
 Sof(F116)=Sof(F117)=Sof(F118)=Sof(C324)=1-FVAR(1)
 Sof(F16)=Sof(F17)=Sof(F18)=Sof(C224)=FVAR(1)
 Sof(F107)=Sof(F108)=Sof(F109)=Sof(C315)=1-FVAR(2)
 Sof(F7)=Sof(F8)=Sof(F9)=Sof(C215)=FVAR(2)
 Sof(F110)=Sof(F111)=Sof(F112)=Sof(C316)=1-FVAR(3)
 Sof(F10)=Sof(F11)=Sof(F12)=Sof(C216)=FVAR(3)
 Sof(F101)=Sof(F102)=Sof(F103)=1-FVAR(4)
 Sof(F1)=Sof(F2)=Sof(F3)=FVAR(4)
 Sof(F104)=Sof(F105)=Sof(F106)=1-FVAR(5)
 Sof(F4)=Sof(F5)=Sof(F6)=FVAR(5)
 Sof(F119)=Sof(F120)=Sof(F121)=Sof(C331)=1-FVAR(6)
 Sof(F19)=Sof(F20)=Sof(F21)=Sof(C231)=FVAR(6)
 Sof(F122)=Sof(F123)=Sof(F124)=Sof(C332)=1-FVAR(7)
 Sof(F22)=Sof(F23)=Sof(F24)=Sof(C232)=FVAR(7)
 Sof(C147)=Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(C148)=Sof(H14D)=Sof(H14E)=
 Sof(H14F)=1-FVAR(8)
 Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(H47C)=Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(H48C)=
 FVAR(8)
 Fixed Sof: O3(0.5) O3A(0.25) O3B(0.25) C2(0.5) C2A(0.25) C2B(0.25)
6.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C13(H13A,H13B), C28(H28A,H28B), C40(H40A,H40B), C43(H43A,H43B)
6.b Aromatic/amide H refined with riding coordinates:
 C25(H25), C202(H202), C204(H204), C206(H206), C210(H210), C212(H212),
 C214(H214), C218(H218), C220(H220), C222(H222), C226(H226), C228(H228),
 C230(H230)
6.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,
 H33B,H33C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C),
 C48(H48A,H48B,H48C), C147(H14A,H14B,H14C), C148(H14D,H14E,H14F)
;