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_4088962
_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         'C28 H42 Cl4 Ir2'
_chemical_formula_sum            'C28 H42 Cl4 Ir2'
_chemical_formula_weight         904.81
_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     direct
_audit_creation_date             2016-04-30
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                99.228(2)
_cell_angle_beta                 109.651(2)
_cell_angle_gamma                96.017(2)
_cell_formula_units_Z            1
_cell_length_a                   8.2486(2)
_cell_length_b                   8.8636(3)
_cell_length_c                   10.6121(3)
_cell_measurement_reflns_used    16798
_cell_measurement_temperature    100.2(8)
_cell_measurement_theta_max      32.1640
_cell_measurement_theta_min      4.1010
_cell_volume                     710.63(4)
_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      100.2(8)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0061
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.941
_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    -83.00  13.00   1.00    3.00    --  -29.69 113.00 -17.00   96
  2  \w   -102.00   3.00   1.00    3.00    --  -29.69 -77.00-120.00  105
  3  \w   -102.00   3.00   1.00    3.00    --  -29.69 -77.00  90.00  105
  4  \w   -102.00   3.00   1.00    3.00    --  -29.69 -77.00-180.00  105
  5  \w    -50.00  44.00   1.00    3.00    --  -29.69  38.00 -30.00   94
  6  \w   -100.00  -6.00   1.00    3.00    --  -29.69 -57.00 -30.00   94
  7  \w   -109.00 -35.00   1.00    3.00    --  -29.69-178.00   0.00   74
  8  \w   -109.00 -35.00   1.00    3.00    --  -29.69-178.00 120.00   74
  9  \w   -100.00  -6.00   1.00    3.00    --  -29.69 -57.00 -90.00   94
 10  \w    -50.00  44.00   1.00    3.00    --  -29.69  38.00-150.00   94
 11  \w   -112.00 -32.00   1.00    3.00    --  -29.69 178.00  90.00   80
 12  \w   -103.00   2.00   1.00    3.00    --  -29.69 -38.00  30.00  105
 13  \w    -53.00  41.00   1.00    3.00    --  -29.69  57.00 120.00   94
 14  \w   -112.00 -87.00   1.00    3.00    --  -29.69 178.00-180.00   25
 15  \w   -102.00   3.00   1.00    3.00    --  -29.69 -77.00  30.00  105
;
_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      0.0636283000
_diffrn_orient_matrix_UB_12      0.0682005000
_diffrn_orient_matrix_UB_13      0.0313407000
_diffrn_orient_matrix_UB_21      0.0075213000
_diffrn_orient_matrix_UB_22      0.0042092000
_diffrn_orient_matrix_UB_23      -0.0640408000
_diffrn_orient_matrix_UB_31      -0.0669513000
_diffrn_orient_matrix_UB_32      0.0458397000
_diffrn_orient_matrix_UB_33      -0.0135413000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.941
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            21939
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.941
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         32.359
_diffrn_reflns_theta_min         3.596
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    9.746
_exptl_absorpt_correction_T_max  0.275
_exptl_absorpt_correction_T_min  0.032
_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    2.114
_exptl_crystal_description       block
_exptl_crystal_F_000             432
_exptl_crystal_size_max          0.643
_exptl_crystal_size_mid          0.407
_exptl_crystal_size_min          0.173
_refine_diff_density_max         1.254
_refine_diff_density_min         -1.337
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     158
_refine_ls_number_reflns         4787
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0179
_refine_ls_R_factor_gt           0.0169
_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^)+(0.0200P)^2^+0.3818P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0410
_refine_ls_wR_factor_ref         0.0415
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4619
_reflns_number_total             4787
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00580_si_002.cif
_cod_data_source_block           2o_lbx-062abs
_cod_original_cell_volume        710.63(3)
_cod_database_code               4088962
_chemical_oxdiff_formula         'C28 H42 Cl4 Ir2'
_chemical_oxdiff_usercomment     'LBI97 @ 100K'
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H6A(0.028) H6B(0.028) H6C(0.028) H7A(0.027) H7B(0.027) H7C(0.027)
 H8A(0.03) H8B(0.03) H8C(0.03) H9A(0.033) H9B(0.033) H9C(0.033) H10(0.021)
 H11A(0.021) H11B(0.021) H12A(0.041) H12B(0.041) H13A(0.042) H13B(0.042)
 H14A(0.035) H14B(0.035)
 Fixed X: H6A(0.9657) H6B(0.8998) H6C(1.0335) H7A(0.9307) H7B(0.7663)
 H7C(0.7634) H8A(0.5536) H8B(0.3972) H8C(0.3989) H9A(0.3427) H9B(0.2915)
 H9C(0.4234) H10(0.5867) H11A(0.8493) H11B(0.9483) H12A(0.9264) H12B(0.959)
 H13A(0.7047) H13B(0.6292) H14A(0.6578) H14B(0.4853)
 Fixed Y: H6A(0.1286) H6B(-0.0159) H6C(0.13) H7A(0.1233) H7B(-0.0146)
 H7C(0.138) H8A(0.3043) H8B(0.1727) H8C(0.35) H9A(0.419) H9B(0.2895)
 H9C(0.4459) H10(0.3398) H11A(0.4495) H11B(0.3478) H12A(0.2958) H12B(0.1641)
 H13A(0.0451) H13B(0.2052) H14A(0.0294) H14B(0.0902)
 Fixed Z: H6A(0.6714) H6B(0.7253) H6C(0.8318) H7A(1.0219) H7B(0.9621)
 H7C(1.0643) H8A(1.0345) H8B(0.9301) H8C(0.9163) H9A(0.7168) H9B(0.5797)
 H9C(0.6029) H10(0.4886) H11A(0.5017) H11B(0.607) H12A(0.348) H12B(0.4377)
 H13A(0.2594) H13B(0.2507) H14A(0.4617) H14B(0.3752)
;
_shelx_res_checksum              1186
_shelx_hkl_checksum              10326
_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 3.156
_oxdiff_exptl_absorpt_empirical_full_min 0.627