Rapid Access to Derivatized, Dimeric, Ring-Substituted Dichloro(cyclopentadienyl)rhodium(III) and Iridium(III) Complexes
Brown, Loren C.; Ressegue, Emily; Merola, Joseph S.; Organometallics 35 (2016) 4014–; doi:10.1021/acs.organomet.6b00580

data_4088959
_publ_section_title
;
 Rapid Access to Derivatized, Dimeric, Ring-Substituted
 Dichloro(cyclopentadienyl)rhodium(III) and Iridium(III) Complexes
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              4014
_journal_paper_doi               10.1021/acs.organomet.6b00580
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         '2(C13 H21 Cl2 Ir)'
_chemical_formula_sum            'C26 H42 Cl4 Ir2'
_chemical_formula_weight         880.79
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-07-09
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 100.5832(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3996(2)
_cell_length_b                   12.52230(17)
_cell_length_c                   17.3680(3)
_cell_measurement_reflns_used    14548
_cell_measurement_temperature    100.1(3)
_cell_measurement_theta_max      32.0800
_cell_measurement_theta_min      3.8740
_cell_volume                     2864.67(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.1(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0061
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.927
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -48.00  40.00   1.00    4.00    --  -29.53  38.00 -30.00   88
  2  \w    -47.00   2.00   1.00    4.00    --  -29.53 -77.00-180.00   49
  3  \w    -65.00 -39.00   1.00    4.00    --  -29.53-178.00-150.00   26
  4  \w    -98.00 -72.00   1.00    4.00    --  -29.53 -77.00-180.00   26
  5  \w   -109.00 -78.00   1.00    4.00    --  -29.53-178.00-150.00   31
  6  \w    -98.00  -6.00   1.00    4.00    --  -29.53 -57.00  60.00   92
  7  \w    -53.00  41.00   1.00    4.00    --  -29.53  57.00-150.00   94
  8  \w    -92.00  -1.00   1.00    4.00    --  -29.53 130.00 -39.69   91
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0172791000
_diffrn_orient_matrix_UB_12      -0.0444453000
_diffrn_orient_matrix_UB_13      -0.0191914000
_diffrn_orient_matrix_UB_21      0.0510010000
_diffrn_orient_matrix_UB_22      0.0157337000
_diffrn_orient_matrix_UB_23      0.0138354000
_diffrn_orient_matrix_UB_31      0.0010849000
_diffrn_orient_matrix_UB_32      -0.0313616000
_diffrn_orient_matrix_UB_33      0.0341591000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_unetI/netI     0.0447
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.927
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            32538
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.927
_diffrn_reflns_theta_full        30.500
_diffrn_reflns_theta_max         32.380
_diffrn_reflns_theta_min         3.705
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    9.668
_exptl_absorpt_correction_T_max  0.417
_exptl_absorpt_correction_T_min  0.063
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
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    2.042
_exptl_crystal_description       plate
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.472
_exptl_crystal_size_mid          0.404
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.848
_refine_diff_density_min         -1.310
_refine_diff_density_rms         0.187
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         9514
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0310
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0239P)^2^+0.8761P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0615
_refine_ls_wR_factor_ref         0.0651
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8062
_reflns_number_total             9514
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00580_si_002.cif
_cod_data_source_block           2f_lbx-071abs
_cod_original_cell_volume        2864.66(8)
_cod_database_code               4088959
_chemical_oxdiff_formula         'C26 H42 Cl4 Ir2'
_chemical_oxdiff_usercomment     ERI10
_reflns_odcompleteness_completeness 99.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H19A(0.04) H19B(0.04) H19C(0.04) H20A(0.041) H20B(0.041)
 H20C(0.041) H21A(0.054) H21B(0.054) H21C(0.054) H22A(0.06) H22B(0.06)
 H22C(0.06) H23(0.042) H24A(0.041) H24B(0.041) H25A(0.059) H25B(0.059)
 H25C(0.059) H26A(0.064) H26B(0.064) H26C(0.064) H6A(0.04) H6B(0.04) H6C(0.04)
 H7A(0.043) H7B(0.043) H7C(0.043) H8A(0.044) H8B(0.044) H8C(0.044) H9A(0.04)
 H9B(0.04) H9C(0.04) H10(0.033) H11A(0.03) H11B(0.03) H12A(0.063) H12B(0.063)
 H12C(0.063) H13A(0.08) H13B(0.08) H13C(0.08)
 Fixed X: H19A(0.1811) H19B(0.2879) H19C(0.2685) H20A(0.3252) H20B(0.3841)
 H20C(0.307) H21A(0.2268) H21B(0.2459) H21C(0.1339) H22A(0.0394) H22B(0.0562)
 H22C(-0.0335) H23(0.0644) H24A(0.1916) H24B(0.1245) H25A(0.013) H25B(0.1259)
 H25C(0.0708) H26A(-0.0598) H26B(-0.0832) H26C(-0.0816) H6A(0.5743) H6B(0.482)
 H6C(0.4748) H7A(0.3117) H7B(0.2319) H7C(0.2359) H8A(0.2089) H8B(0.1914)
 H8C(0.2519) H9A(0.3807) H9B(0.4459) H9C(0.5013) H10(0.6465) H11A(0.5718)
 H11B(0.564) H12A(0.754) H12B(0.7394) H12C(0.7035) H13A(0.6437) H13B(0.7387)
 H13C(0.6535)
 Fixed Y: H19A(0.3543) H19B(0.4114) H19C(0.3488) H20A(0.4221) H20B(0.5331)
 H20C(0.516) H21A(0.6769) H21B(0.7708) H21C(0.7489) H22A(0.7888) H22B(0.7882)
 H22C(0.7192) H23(0.4559) H24A(0.5488) H24B(0.6551) H25A(0.5795) H25B(0.5681)
 H25C(0.4673) H26A(0.6385) H26B(0.5243) H26C(0.5379) H6A(0.2893) H6B(0.3711)
 H6C(0.2538) H7A(0.2045) H7B(0.2702) H7C(0.1427) H8A(0.0922) H8B(0.201)
 H8C(0.1044) H9A(0.1571) H9B(0.2647) H9C(0.1529) H10(0.2754) H11A(0.4426)
 H11B(0.4385) H12A(0.439) H12B(0.4505) H12C(0.5447) H13A(0.2713) H13B(0.2552)
 H13C(0.1645)
 Fixed Z: H19A(0.7579) H19B(0.7882) H19C(0.7065) H20A(0.6075) H20B(0.625)
 H20C(0.544) H21A(0.5118) H21B(0.5753) H21C(0.5274) H22A(0.6171) H22B(0.7107)
 H22C(0.6607) H23(0.7894) H24A(0.8668) H24B(0.8584) H25A(0.9304) H25B(0.9795)
 H25C(0.9333) H26A(0.7743) H26B(0.8083) H26C(0.7169) H6A(0.4748) H6B(0.4514)
 H6C(0.4144) H7A(0.402) H7B(0.4415) H7C(0.4477) H8A(0.574) H8B(0.618)
 H8C(0.6658) H9A(0.7524) H9B(0.7662) H9C(0.7588) H10(0.597) H11A(0.5899)
 H11B(0.6806) H12A(0.6285) H12B(0.7175) H12C(0.6563) H13A(0.7579) H13B(0.715)
 H13C(0.7093)
;
_shelx_res_checksum              30087
_shelx_hkl_checksum              20710
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.249
_oxdiff_exptl_absorpt_empirical_full_min 0.747