Iridium Complexes of the Conformationally Rigid IBioxMe4 Ligand: Hydride Complexes and Dehydrogenation of Cyclooctene
Hauser, Simone A.; Tonner, Ralf; Chaplin, Adrian B.; Organometallics 34 (2015) 4419–; doi:10.1021/acs.organomet.5b00658

data_4087869
_publ_section_title
;
 Iridium Complexes of the Conformationally Rigid IBioxMe4 Ligand: Hydride
 Complexes and Dehydrogenation of Cyclooctene
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              4419
_journal_paper_doi               10.1021/acs.organomet.5b00658
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C26 H40 Ir N4 O4, C32 H12 B F24'
_chemical_formula_sum            'C58 H52 B F24 Ir N4 O4'
_chemical_formula_weight         1528.04
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-06-17
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 112.3623(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.9906(2)
_cell_length_b                   18.4566(3)
_cell_length_c                   19.5861(2)
_cell_measurement_reflns_used    26864
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      34.1750
_cell_measurement_theta_min      3.2980
_cell_volume                     6014.39(15)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.2833
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega   39.00   87.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       23.3155  178.0000  120.0000 48

  2 omega   39.00   88.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       23.3155  178.0000   30.0000 49

  3 omega  -38.00    5.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.4093  -57.0000 -180.0000 43

  4 omega  -61.00    9.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.4093  -77.0000  150.0000 70

  5 omega  -86.00  -60.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.4093  -38.0000    0.0000 26

  6 omega -101.00  -45.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.4093  -77.0000   90.0000 56

  7 omega  -95.00  -55.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.4093  -57.0000 -180.0000 40

  8 omega -114.00  -64.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.4093 -178.0000  -30.0000 50

  9 omega  -51.00   51.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.4093   38.0000 -180.0000 102
;
_diffrn_measurement_device_type  'Oxford Diffraction: Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0211573000
_diffrn_orient_matrix_UB_12      -0.0054645000
_diffrn_orient_matrix_UB_13      -0.0384087000
_diffrn_orient_matrix_UB_21      0.0250815000
_diffrn_orient_matrix_UB_22      0.0257748000
_diffrn_orient_matrix_UB_23      -0.0076131000
_diffrn_orient_matrix_UB_31      0.0272073000
_diffrn_orient_matrix_UB_32      -0.0279884000
_diffrn_orient_matrix_UB_33      0.0004992000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0371
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            62393
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        27.103
_diffrn_reflns_theta_max         27.103
_diffrn_reflns_theta_min         3.055
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.344
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70722
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.688
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3032
_exptl_crystal_recrystallization_method
'Crystals grown from C6H4F2-heptane at 293 K'
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.092
_refine_diff_density_min         -0.661
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     865
_refine_ls_number_reflns         13246
_refine_ls_number_restraints     246
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0306
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0296P)^2^+9.1737P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0690
_refine_ls_wR_factor_ref         0.0719
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11596
_reflns_number_total             13246
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00658_si_003.cif
_cod_data_source_block           0070abc14
_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_original_cell_volume        6014.37(14)
_cod_database_code               4087869
_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
 C208-F4 \\sim C208-F5 \\sim C208-F6 \\sim C208-F4A \\sim C208-F5A \\sim
C208-F6A
 with sigma of 0.01
 F4-F5 \\sim F5-F6 \\sim F6-F4 \\sim F4A-F5A \\sim F5A-F6A \\sim F6A-F4A
 with sigma of 0.01
 C205-F4 \\sim C205-F5 \\sim C205-F6 \\sim C205-F4A \\sim C205-F5A \\sim
C205-F6A
 with sigma of 0.01
 C223-F13 \\sim C223-F14 \\sim C223-F15
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
F1 \\sim F2 \\sim F3 \\sim F4 \\sim F4A \\sim F5 \\sim F5A \\sim F6 \\sim F6A
\\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: 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(F4A) \\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(F5A) \\sim Ueq, Uanis(F6)
\\sim Ueq, Uanis(F6A) \\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: with sigma of 0.007 and sigma for
terminal atoms of 0.02
4. Others
 Sof(F4A)=Sof(F5A)=Sof(F6A)=1-FVAR(1)
 Sof(F4)=Sof(F5)=Sof(F6)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C12(H12A,H12B), C15(H15A,
 H15B), C27(H27A,H27B), C30(H30A,H30B)
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)
5.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,
 H35B,H35C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'