Rhodium(I) and Iridium(I) Complexes of the Conformationally Rigid IBioxMe4 Ligand: Computational and Experimental Studies of Unusually Tilted NHC Coordination Geometries
Luy, Jan-Niclas; Hauser, Simone A.; Chaplin, Adrian B.; Tonner, Ralf; Organometallics 34 (2015) 5099–; doi:10.1021/acs.organomet.5b00692

data_4087905
_publ_section_title
;
 Rhodium(I) and Iridium(I) Complexes of the Conformationally Rigid
 IBioxMe4 Ligand: Computational and Experimental Studies of Unusually
 Tilted NHC Coordination Geometries
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              5099
_journal_paper_doi               10.1021/acs.organomet.5b00692
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C51 H72 N6 O6 Rh, C32 H12 B F24'
_chemical_formula_sum            'C83 H84 B F24 N6 O6 Rh'
_chemical_formula_weight         1831.28
_chemical_melting_point          ?
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-01-21
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.19 svn.r3143 for OlexSys, GUI svn.r4992)
;
_cell_angle_alpha                90
_cell_angle_beta                 110.6897(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.8658(4)
_cell_length_b                   14.75921(19)
_cell_length_c                   26.5909(4)
_cell_measurement_reflns_used    23289
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.9550
_cell_measurement_theta_min      2.5900
_cell_volume                     8028.0(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_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      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2833
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -56.00   57.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       23.1653  -77.0000  150.0000 113

  2 omega  -25.00   65.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       23.1653  -99.0000  -60.0000 90

  3 omega  -66.00  113.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       23.1653    0.0000  -30.0000 179

  4 omega   -3.00   99.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       23.1653   38.0000 -120.0000 102

  5 omega  -57.00    1.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.2590  -77.0000  -60.0000 58

  6 omega  -74.00  -27.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.2590  127.0000   -2.0000 47
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction: Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0174721000
_diffrn_orient_matrix_UB_12      -0.0365293000
_diffrn_orient_matrix_UB_13      -0.0058684000
_diffrn_orient_matrix_UB_21      0.0185484000
_diffrn_orient_matrix_UB_22      0.0311227000
_diffrn_orient_matrix_UB_23      -0.0090803000
_diffrn_orient_matrix_UB_31      0.0235170000
_diffrn_orient_matrix_UB_32      0.0025897000
_diffrn_orient_matrix_UB_33      0.0263860000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0697
_diffrn_reflns_av_unetI/netI     0.0492
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            93159
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.681
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         2.934
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.326
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82562
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3752
_exptl_crystal_recrystallization_method
'Crystals grown from 1,2-C6H4F2-heptane at 293 K'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.108
_refine_diff_density_min         -0.644
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1108
_refine_ls_number_reflns         15214
_refine_ls_number_restraints     312
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0712
_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^)+(0.0839P)^2^+4.9722P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1371
_refine_ls_wR_factor_ref         0.1507
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11769
_reflns_number_total             15214
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00692_si_003.cif
_cod_data_source_block           0138abc15
_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               4087905
_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
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
 C223-F13 \\sim C223-F14 \\sim C223-F15 \\sim C223-F113 \\sim C223-F114 \\sim
C223-F115
 with sigma of 0.01
 F13-F14 \\sim F14-F15 \\sim F15-F13 \\sim F113-F114 \\sim F114-F115 \\sim
F115-F113
 with sigma of 0.01
 C219-F13 \\sim C219-F14 \\sim C219-F15 \\sim C219-F113 \\sim C219-F114 \\sim
C219-F115
 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 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 F113 \\sim F114 \\sim F115: 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(F113) \\sim Ueq,
Uanis(F114) \\sim Ueq, Uanis(F115) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(F3) = Uanis(F102)
Uanis(F101) = Uanis(F2)
Uanis(F103) = Uanis(F1)
Uanis(F15) = Uanis(F113)
Uanis(F114) = Uanis(F13)
Uanis(F14) = Uanis(F115)
4. Others
 Fixed Sof: F1(0.5) F2(0.5) F3(0.5) F13(0.5) F14(0.5) F15(0.5) F101(0.5)
 F102(0.5) F103(0.5) F113(0.5) F114(0.5) F115(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C11(H11A,H11B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B),
 C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B),
  C21(H21A,H21B), C22(H22A,H22B), C29(H29A,H29B), C32(H32A,H32B), C34(H34A,
 H34B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B),
 C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B),
  C50(H50A,H50B), C53(H53A,H53B), C55(H55A,H55B), C56(H56A,H56B), C57(H57A,
 H57B), C58(H58A,H58B), C59(H59A,H59B), C60(H60A,H60B), C61(H61A,H61B),
 C62(H62A,H62B), C63(H63A,H63B), C64(H64A,H64B)
5.b Aromatic/amide H refined with riding coordinates:
 C202(H202), C204(H204), C206(H206), C210(H210), C212(H212), C214(H214),
 C218(H218), C220(H220), C222(H222), C226(H226), C228(H228), C230(H230)
;
_olex2_submission_special_instructions 'No special instructions were received'