Metallocene to metallocene conversion. Synthesis of an oxazoline-substituted pentamethyliridocenium cation from a ferrocenyloxazoline
Ross A. Arthurs; Peter N. Horton; Simon J. Coles; Christopher J. Richards; Chem.Commun. 52 (2016) 7024–; doi:

data_7119141
_publ_section_title
;
 Metallocene to metallocene conversion. Synthesis of an
 oxazoline-substituted pentamethyliridocenium cation from a
 ferrocenyloxazoline
;
_journal_name_full               Chem.Commun.
_journal_page_first              7024
_journal_volume                  52
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C21 H29 Ir N O, F6 P'
_chemical_formula_sum            'C21 H29 F6 Ir N O P'
_chemical_formula_weight         648.62
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-12-16 deposited with the CCDC.
2016-04-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.0929(2)
_cell_length_b                   15.6774(4)
_cell_length_c                   20.8647(5)
_cell_measurement_reflns_used    9814
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5120
_cell_measurement_theta_min      2.3280
_cell_volume                     2320.12(10)
_computing_cell_refinement
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
;
_computing_data_collection
;
Rigaku CrystalClear-SM Expert 3.1 b27
;
_computing_data_reduction
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material
;
 WINGX (Farrugia, 1998)
 Olex2 (Dolomanov et al., 2009)
;
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis, 2007'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'four-circle \k diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMesh'
_diffrn_radiation_collimation    'Confocal mirrors, VHF Varimax '
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0298
_diffrn_reflns_av_unetI/netI     0.0326
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            15356
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.479
_diffrn_reflns_theta_min         2.345
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    5.884
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69730
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'Pale Yellow'
_exptl_crystal_density_diffrn    1.857
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.901
_refine_diff_density_min         -0.432
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details
;
 Flack x determined using 1915 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.007(6)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         5262
_refine_ls_number_restraints     616
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0333
_refine_ls_R_factor_gt           0.0281
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0338P)^2^+0.7157P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0590
_refine_ls_wR_factor_ref         0.0606
_reflns_Friedel_coverage         0.733
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.971
_reflns_number_gt                4842
_reflns_number_total             5262
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc01959e2.cif
_cod_data_source_block           3
_cod_database_code               7119141
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.321
_shelx_estimated_absorpt_t_max   0.944
_shelx_res_checksum              12608