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_4088958
_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         'C26 H42 Cl4 Ir2'
_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             2016-05-11
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 97.759(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.88539(19)
_cell_length_b                   16.9849(5)
_cell_length_c                   10.7692(3)
_cell_measurement_reflns_used    6302
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      31.9540
_cell_measurement_theta_min      4.0000
_cell_volume                     1429.14(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0061
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measurement_details
;
  1 omega -112.00  -84.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  178.0000 -180.0000 28

  2 omega  -50.00   37.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315   38.0000 -150.0000 87

  3 omega -103.00    1.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  -38.0000   30.0000 104

  4 omega -107.00  -51.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315 -178.0000  120.0000 56

  5 omega  -41.00   43.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315   38.0000  -30.0000 84

  6 omega  -92.00  -37.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315 -178.0000  -90.0000 55

  7 omega  -92.00  -47.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  129.0000   29.3029 45
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0442625000
_diffrn_orient_matrix_UB_12      -0.0038003000
_diffrn_orient_matrix_UB_13      -0.0615824000
_diffrn_orient_matrix_UB_21      0.0509762000
_diffrn_orient_matrix_UB_22      -0.0331819000
_diffrn_orient_matrix_UB_23      -0.0101957000
_diffrn_orient_matrix_UB_31      -0.0608726000
_diffrn_orient_matrix_UB_32      -0.0249944000
_diffrn_orient_matrix_UB_33      0.0228119000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0473
_diffrn_reflns_av_unetI/netI     0.0547
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.930
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            15220
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.930
_diffrn_reflns_theta_full        30.000
_diffrn_reflns_theta_max         32.376
_diffrn_reflns_theta_min         3.543
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    9.689
_exptl_absorpt_correction_T_max  0.597
_exptl_absorpt_correction_T_min  0.242
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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    2.047
_exptl_crystal_description       irregular
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.2982
_exptl_crystal_size_mid          0.1502
_exptl_crystal_size_min          0.0766
_refine_diff_density_max         2.089
_refine_diff_density_min         -1.161
_refine_diff_density_rms         0.222
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         4766
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0346
_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^)+(0.0221P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0605
_refine_ls_wR_factor_ref         0.0649
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3901
_reflns_number_total             4766
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00580_si_002.cif
_cod_data_source_block           2e_lbx-024abs
_cod_original_cell_volume        1429.15(6)
_cod_database_code               4088958
_chemical_oxdiff_formula         'C26 H42 Cl4 Ir2'
_reflns_odcompleteness_completeness 99.67
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H6A(0.034) H6B(0.034) H6C(0.034) H7A(0.042) H7B(0.042) H7C(0.042)
 H8A(0.038) H8B(0.038) H8C(0.038) H9A(0.036) H9B(0.036) H9C(0.036) H10A(0.02)
 H10B(0.02) H11(0.023) H12A(0.029) H12B(0.029) H12C(0.029) H13A(0.047)
 H13B(0.047) H13C(0.047)
 Fixed X: H6A(0.656) H6B(0.5212) H6C(0.5016) H7A(0.5351) H7B(0.6406)
 H7C(0.6747) H8A(0.2028) H8B(0.2497) H8C(0.397) H9A(-0.0428) H9B(0.0278)
 H9C(0.0768) H10A(0.2992) H10B(0.1695) H11(-0.0326) H12A(-0.0582) H12B(-0.1237)
 H12C(0.0611) H13A(0.1873) H13B(0.0066) H13C(0.1657)
 Fixed Y: H6A(0.7524) H6B(0.7952) H6C(0.802) H7A(0.6216) H7B(0.5656)
 H7C(0.6585) H8A(0.5016) H8B(0.456) H8C(0.4775) H9A(0.5723) H9B(0.5885)
 H9C(0.5086) H10A(0.767) H10B(0.6985) H11(0.7474) H12A(0.7848) H12B(0.8547)
 H12C(0.8599) H13A(0.8815) H13B(0.8697) H13C(0.8151)
 Fixed Z: H6A(0.3066) H6B(0.3825) H6C(0.233) H7A(0.0467) H7B(0.149)
 H7C(0.1524) H8A(0.0888) H8B(0.2189) H8C(0.1359) H9A(0.2873) H9B(0.4314)
 H9C(0.3659) H10A(0.4912) H10B(0.5169) H11(0.3477) H12A(0.556) H12B(0.4619)
 H12C(0.5437) H13A(0.3412) H13B(0.2559) H13C(0.2349)
;
_shelx_res_checksum              39133
_shelx_hkl_checksum              99217
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'